CN101665990A - Fibroin blending regeneration cellulose fiber and preparation technique thereof - Google Patents

Abstract

The invention discloses a fibroin blending regeneration cellulose fiber and a preparation technique thereof. The inventive technique comprises the following steps: (1) preparing nano level fibroin powder, and (2) preparing cellulose fiber. Compared with the prior art, the invention has the following beneficial effects: the invention overcomes the difficulty of superfining smash of fibroin powder and adopts self-developed nano smashing equipment, and the grain diameter of the produced fibroin powder is within 50-500 nano with the rate being 100%; the invention can realize 50 tons of nano levelfibroin powder in terms of annual yield, meets the market demand, and has larger market value; and the invention can used in application of nano level fibroin powder in fabric after completing nano fibroin powder smashing equipment.

Description

Fibroin blending regeneration cellulose fiber and preparation technology thereof

Technical field

The invention belongs to the cellulose fibre technical field, more specifically relate to a kind of fibroin blending regeneration cellulose fiber and preparation technology thereof.

Background technology

The market scale of whole world fibroin industry is at 50～6,000,000,000 dollars, and silk fibroin powder accounts for 50% share, and its range of application is more extensive, and is running stores, will reach more than 10,000,000,000 in 3 years its market scales.

Aspect processing, based on Japan, its Application Areas spreads all over medicines and health protection, food and beauty industry to fibroin at present, and major product has cosmetics, health food, and technical merit is also led over other country.Make that its added value of product is high.China through the number development of decades, has now become the fibroin place of production very important on the silk market, the world since new China sets up, the main place of production is Zhejiang and Jiangsu two provinces.But the high-quality fibroin of China is few, and added value is low.

The market overall situation is badly in need of the appearance of super-refinement silk fibroin powder.100 nanometers are 1/75th of human body face pores, very easily absorb.Fibroin contains 19 seed amino acids because of it; nearly 20 kinds of mineral matters; the high-activity biological taurine; abundant fibroin and a large amount of trace elements; can improve the activity of flight against senium of human body factor S OD and amino acid carrier GSH-PX, the effect with the arresting convulsion of calming the nerves, clearing heat and detoxicating, thin protecting liver, coordinating intestines and stomach, additional calcium system, microelement-supplementing for oral administration.External application energy delaying skin aging, removing beverage, anti-acne, crease-resistant strengthen multiple efficacies such as skin gloss and elasticity.The appearance of nano-grade silk albumen powder makes the practical application of silk fibroin powder aspect beauty and health care obtain the raising of the order of magnitude.

There are two kinds of silk fibroin powders, micron order silk fibroin powder and nano-grade silk albumen powder now on the domestic and international market.

Traditional preparation technology can make the silk fibroin powder of 3-10um, and particle diameter is big, and absorptivity is low, and its process energy consumption is big, the production cost height, and nutrition in the fibroin is damaged or dissolves.After testing, the only surplus 3-6 kind of the silk fibroin powder after traditional chemical method preparation technology makes, amino acid, because of product particle is many more than 5um, absorptivity is low simultaneously.

The micron order silk fibroin powder is applied to cosmetic health product all the time, but because of its particle is big, difficult absorption, process can be lost the part nutritional labeling, so its application continuously effective fruit is not good, and constantly problems such as bad reaction are taken in appearance orally.

New technology fibroin manufacture method is divided into physics method and chemical method.The nanometer silk fibroin powder that physical method makes is slightly soluble in water, do not change itself solid state properties, and can 100% keep the original composition and the nutrient of silk fibroin powder, and the solvable nanometer silk fibroin powder that makes with chemical method, human body absorbs easily, but because passed through chemical treatment, the silk fibroin powder self component has had change.Concrete more as shown in table 1.

Silk fibroin powder is in technologic breakthrough, and its particle diameter is promoted to nanoscale from micron order, and it is used also from flush coat, and the is oral beauty functions of Denging is developed to new material functions such as being used for weaving face fabric.

Fibroin fiber is a kind of novel functional textile material, has vast market prospect.The fibroin fiber textiles of pushing the domestic market at present to has progressively extended to fields such as shirt, outdoor activity clothing, jean, socks and bedding from initial knitted underwear, brassiere, T-shirt, pants etc., supply falls short of demand for product.The health care of fibroin fiber uniqueness has caused external travelling trader's concern equally.

Fibroin fiber is the fiber of being made by fibroin powder and the spinning of viscose pulp dope blending, is the gang of new function fiber, because of it has better spinnability, can become the textile raw material of all size with various natural and synthetic fiber blending.

But with regard to present prior art, among the preparation technology, key technologies such as reunion of fibroin powder and slurry stability still have to be solved.

Summary of the invention

The objective of the invention is to overcome the deficiencies in the prior art, a kind of fibroin blending regeneration cellulose fiber is provided.

Another object of the present invention is to provide the preparation method of this fibroin blending regeneration cellulose fiber.

For achieving the above object, the present invention has taked following technical scheme:

The preparation technology of fibroin blending regeneration cellulose fiber comprises the steps:

(1) preparation of nano-grade silk albumen powder;

(2) preparation of cellulose fibre.

In the technique scheme, the preparation of described nano-grade silk albumen powder comprises the steps:

(a) fibroin is through behind the elevator, and coarse fodder enters feed bin;

(b) after air-flow is pulverized, get the meal of 5 μ m～10 μ m;

(c) behind the meal feeding warehouse, through the dried-air drier drying;

(d) entering cryogenic turbo pressurized air stream pulverizer pulverizes;

(e) after one-level classification, secondary classification, get the silk fibroin powder of 50nm～100nm.

In the technique scheme, the preparation of described cellulose fibre comprises the preparation of viscose filament yarn and the preparation of viscose staple fibre and tow respectively.

In the technique scheme, the preparation technology of described viscose filament yarn comprises the steps:

(a) mix the dregs of rice after feeding the dregs of rice, dipping, carry out assistant soakage, squeezing, pulverizing;

(b) after experienced, cooling and yellow, dissolve respectively;

(c) mix behind the adding nano-grade silk albumen powder;

(d) filter the back deaeration through filtration together, two roads respectively;

(e) after three roads filtered, continuous spinning was molded into tube;

(f) after finished product inspection, packing gets product.

As improvement of the technical scheme, the continuous spinning in described (e) step is molded into tube and comprises spinning moulding respectively, washes, oils, dries and be wound into a step.

In the technique scheme, described acid bath technological process is: respectively through arriving kerve again after bucket, filtration, the degassing in the middle of acid bath kerve, head tank, spinning machine, the acid bath;

A described water conservancy project process flow of washing is: soft water after washing a water storage tank, baffle heater, head tank, spinning machine, containing zinc water dump tank again to containing the zinc water treatment station;

Described oven dry water conservancy project process flow is: behind soft water drying water buffer barrel, water pump, spinning machine, the steam-water injection to buffer barrel;

Described technology with the cooling system flow process is: NaCl salt solution through distribution reservoir, brine tank, brine pump, screw salt solution machine combination evaporimeter, mix with or the ripe workshop of idle call after to (backwater) brine tank;

Described spinning idle call cold flow journey is: cold water behind back pool, water supply pump, electronic descaling device, steam double-effect lithium bromide unit evaporimeter, spinning air conditioning room, (backwater) filter to back pool;

Described air-conditioning man's process flow is: after the air filter, after heating, chilled water or air cooling, enter atmosphere behind pressure fan, workshop, exhaust blower, toxin expelling tower.

In the technique scheme, the preparation technology of described viscose staple fibre and tow comprises the steps:

(a) mix the dregs of rice and carry out experiencedly through dipping, squeezing, after pulverizing, wind send, carry out yellow after cooling and the weighing;

(b) behind the continuous-dissolution, behind temperature adjustment, pre-deaeration, carry out I road KKF and filter;

(c) carrying out the II road behind temperature adjustment, the rapidly defoaming filters;

(d) fine hair moulding after spinning, drawing-off, the cut-out;

(e) disacidify washing, desulfurization, washing, bleaching;

(f) wash, oil, wet shredding, wind get product after sending, packing.

In the technique scheme, the workflow at alkali station is: liquid caustic soda carries out yellow through new liquid allotment post precipitation; Wherein, a solid caustic soda dissolving back part enters new liquid allotment precipitation, and another part is the concentrated base precipitation; New liquid allotment precipitation gets pressed liquor behind dipping, more after filtering, flood allotment.

In the technique scheme, the workflow at acid station is: spinning is reclaimed and enter tempering tank behind prefiltration, enters kerve and circulating pump more respectively; Behind graphite heater, head tank, enter spinning machine successively behind the quartz sand filtration.

Compared with prior art, the present invention has following beneficial effect:

The present invention has overcome the problem of silk fibroin powder pulverizing super-refinement difficulty, adopts the broken equipment of nanometer of research and development voluntarily, and the silk fibroin powder particle diameter of production reaches 100% in 50～100 nanometers with interior; Can finish 10 tons of nano-grade silk albumen powder annual productions, the demand of having catered to market has very big market value.And after finishing nanometer silk fibroin powder disintegrating apparatus, research nanometer fibroin fiber is in the application of weaving face fabric.It is as a kind of functional fabric, and it had both had, and the gorgeous cunning of light of fibroin is glutinous, the feature and the function of anti-skin-protecting face nursing, and the splendid spinning property of viscose acetal fibre and nearly all textile material blending are arranged again, and range of application is very wide.By project implementation, can develop the high efficient cryogenic air-flow disintegrating apparatus and the production technology that silk fibroin powder are crushed to 50～100 nanometers, can improve area, Jiangsu and Zhejiang Provinces fibroin added value, and the new purposes of developing silk fibroin powder, bigger society and economic implications had.

Description of drawings

Fig. 1 is preparation technology's flow chart of nano-grade silk albumen powder;

Fig. 2 is preparation technology's flow chart of viscose filament yarn;

Fig. 3 is the acid bath process chart;

Fig. 4 is for washing a water conservancy project process flow figure;

Fig. 5 is oven dry water conservancy project process flow figure;

Fig. 6 is technology cooling system flow chart;

Fig. 7 is the cold flow chart of spinning idle call;

Fig. 8 is the air-conditioning process chart;

Fig. 9 is preparation technology's flow chart of viscose staple fibre and tow;

Figure 10 is the workflow diagram at alkali station;

Figure 11 is the workflow diagram at acid station.

The specific embodiment

The invention will be further described below in conjunction with Figure of description and embodiment, but the present invention's scope required for protection is not limited thereto the scope that embodiment is described.

Embodiment 1

The preparation technology of fibroin blending regeneration cellulose fiber comprises the steps:

(1) preparation of nano-grade silk albumen powder;

(2) preparation of cellulose fibre.

Fig. 1 is preparation technology's flow chart of nano-grade silk albumen powder, and as shown in Figure 1: the preparation of described nano-grade silk albumen powder comprises the steps:

(a) fibroin is through behind the elevator, and coarse fodder enters feed bin;

(b) after air-flow is pulverized, get the meal of 5 μ m～10 μ m;

(c) behind the meal feeding warehouse, through the dried-air drier drying;

(d) entering cryogenic turbo pressurized air stream pulverizer pulverizes;

(e) after one-level classification, secondary classification, get the silk fibroin powder of 50nm～100nm.

Silk fibroin powder as raw material can be published in " Science and Technology of food industry " by Zhou Fengjuan, Xu Shiying, Yang Ruijin, the Wang Zhang of Southern Yangtze University's Foodstuffs Academy, and 2003 the 10th phases " solubility silk fibroin powder production new technique " prepares.

Compare with pulverizer commonly used, the nanometer fibroin of design is pulverized machine in the design of the selection of the design of nozzle arrangements, cryogenic coolant and cooling means voluntarily, all has one's own knack.

In the technique scheme, the preparation of described cellulose fibre comprises the preparation of viscose filament yarn and the preparation of viscose staple fibre and tow respectively.

The technical indicator of nano-grade silk albumen powder is as shown in table 2.

Fig. 2 is preparation technology's flow chart of viscose filament yarn, and as shown in Figure 2: the preparation technology of described viscose filament yarn comprises the steps:

(a) mix the dregs of rice after feeding the dregs of rice, dipping, carry out assistant soakage, squeezing, pulverizing;

(b) after experienced, cooling and yellow, dissolve respectively;

(c) mix behind the adding nano-grade silk albumen powder;

(d) filter the back deaeration through filtration together, two roads respectively;

(e) after three roads filtered, continuous spinning was molded into tube;

(f) after finished product inspection, packing gets product.

As improvement of the technical scheme, the continuous spinning in described (e) step is molded into tube and comprises spinning moulding respectively, washes, oils, dries and be wound into a step.

The preparation technology parameter of viscose filament yarn is as shown in table 3.

Fig. 3 is the acid bath process chart; As shown in Figure 3: described acid bath technological process is: respectively through arriving kerve again after bucket, filtration, the degassing in the middle of acid bath kerve, head tank, spinning machine, the acid bath;

Fig. 4 is for washing a water conservancy project process flow figure; As shown in Figure 4: a described water conservancy project process flow of washing is: soft water after washing a water storage tank, baffle heater, head tank, spinning machine, containing zinc water dump tank again to containing the zinc water treatment station;

Fig. 5 is oven dry water conservancy project process flow figure; As shown in Figure 5: described oven dry water conservancy project process flow is: behind soft water drying water buffer barrel, water pump, spinning machine, the steam-water injection to buffer barrel;

Fig. 6 is technology cooling system flow chart; As shown in Figure 6: described technology with the cooling system flow process is: NaCl salt solution through distribution reservoir, brine tank, brine pump, screw salt solution machine combination evaporimeter, mix with or the ripe workshop of idle call after to (backwater) brine tank;

Fig. 7 is the cold flow chart of spinning idle call; As shown in Figure 7: described spinning idle call cold flow journey is: cold water behind back pool, water supply pump, electronic descaling device, steam double-effect lithium bromide unit evaporimeter, spinning air conditioning room, (backwater) filter to back pool;

Fig. 8 is the air-conditioning process chart; As shown in Figure 8: described air-conditioning man's process flow is: after the air filter, after heating, chilled water or air cooling, enter atmosphere behind pressure fan, workshop, exhaust blower, toxin expelling tower.

Fig. 9 is preparation technology's flow chart of viscose staple fibre and tow; As shown in Figure 9: the preparation technology of described viscose staple fibre and tow comprises the steps:

(a) mix the dregs of rice and carry out experiencedly through dipping, squeezing, after pulverizing, wind send, carry out yellow after cooling and the weighing;

(b) behind the continuous-dissolution, behind temperature adjustment, pre-deaeration, carry out I road KKF and filter;

(c) carrying out the II road behind temperature adjustment, the rapidly defoaming filters;

(d) fine hair moulding after spinning, drawing-off, the cut-out;

(e) disacidify washing, desulfurization, washing, bleaching;

(f) wash, oil, wet shredding, wind get product after sending, packing.

The preparation technology parameter of viscose staple fibre and tow is as shown in table 4.

Figure 10 is the workflow diagram at alkali station; As shown in figure 10: the workflow at alkali station is: liquid caustic soda carries out yellow through new liquid allotment post precipitation; Wherein, a solid caustic soda dissolving back part enters new liquid allotment precipitation, and another part is the concentrated base precipitation; New liquid allotment precipitation gets pressed liquor behind dipping, more after filtering, flood allotment.

Figure 11 is the workflow diagram at acid station, and as shown in figure 11: the workflow at acid station is: spinning is reclaimed and enter tempering tank behind prefiltration, enters kerve and circulating pump more respectively; Behind graphite heater, head tank, enter spinning machine successively behind the quartz sand filtration.

Table 1: existing fibroin manufacture method relatively

Table 2: the technical indicator of nano-grade silk albumen powder

Sequence number	Title	Index
			??1	Particle diameter	The 50-100 nanometer
??2	Solubility	??4％
			??3	Moisture	??＜2％
??4	Calcium	??≥360g/kg
			??5	Plumbous	??≤0.5mg/kg
??6	Arsenic	??≤0.5mg/kg
			??7	Protein	??＞1.2％
??8	Total plate count	??≤1000cfu/g
			??9	Yeast and mould	??≤50cfu/g
??10	Coliform	??≤40MPN/100g
			??11	Pathogenic bacteria	Must not detect

Table 3: the preparation technology parameter table of viscose filament yarn

Table 4: the preparation technology parameter table of viscose staple fibre and tow

Claims (10)

1. the preparation technology of fibroin blending regeneration cellulose fiber is characterized in that comprising the steps:

(1) preparation of nano-grade silk albumen powder;

(2) preparation of cellulose fibre.

2. the preparation technology of fibroin blending regeneration cellulose fiber according to claim 1, it is characterized in that: the preparation of described nano-grade silk albumen powder comprises the steps:

(a) fibroin is through behind the elevator, and coarse fodder enters feed bin;

(b) after air-flow is pulverized, get the meal of 5 μ m～10 μ m;

(c) behind the meal feeding warehouse, through the dried-air drier drying;

(d) entering cryogenic turbo pressurized air stream pulverizer pulverizes;

(e) after one-level classification, secondary classification, get the silk fibroin powder of 50nm～100nm.

3. the preparation technology of fibroin blending regeneration cellulose fiber according to claim 1, it is characterized in that: the preparation of described cellulose fibre comprises the preparation of viscose filament yarn and the preparation of viscose staple fibre and tow respectively.

4. the preparation technology of fibroin blending regeneration cellulose fiber according to claim 3, it is characterized in that: the preparation technology of described viscose filament yarn comprises the steps:

(a) mix the dregs of rice after feeding the dregs of rice, dipping, carry out assistant soakage, squeezing, pulverizing;

(b) after experienced, cooling and yellow, dissolve respectively;

(c) mix behind the adding nano-grade silk albumen powder;

(d) filter the back deaeration through filtration together, two roads respectively;

(e) after three roads filtered, continuous spinning was molded into tube;

(f) after finished product inspection, packing gets product.

5. the preparation technology of fibroin blending regeneration cellulose fiber according to claim 4 is characterized in that: the continuous spinning in described (e) step is molded into tube and comprises spinning moulding respectively, washes, oils, dries and be wound into a step.

6. the preparation technology of fibroin blending regeneration cellulose fiber according to claim 4 is characterized in that:

Described acid bath technological process is: respectively through arriving kerve again after bucket, filtration, the degassing in the middle of acid bath kerve, head tank, spinning machine, the acid bath;

A described water conservancy project process flow of washing is: soft water after washing a water storage tank, baffle heater, head tank, spinning machine, containing zinc water dump tank again to containing the zinc water treatment station;

Described oven dry water conservancy project process flow is: behind soft water drying water buffer barrel, water pump, spinning machine, the steam-water injection to buffer barrel;

Described technology with the cooling system flow process is: NaCl salt solution through distribution reservoir, brine tank, brine pump, screw salt solution machine combination evaporimeter, mix with or the ripe workshop of idle call after to (backwater) brine tank;

Described spinning idle call cold flow journey is: cold water behind back pool, water supply pump, electronic descaling device, steam double-effect lithium bromide unit evaporimeter, spinning air conditioning room, (backwater) filter to back pool;

Described air-conditioning man's process flow is: after the air filter, after heating, chilled water or air cooling, enter atmosphere behind pressure fan, workshop, exhaust blower, toxin expelling tower.

7. the preparation technology of fibroin blending regeneration cellulose fiber according to claim 3, it is characterized in that: the preparation technology of described viscose staple fibre and tow comprises the steps:

(a) mix the dregs of rice and carry out experiencedly through dipping, squeezing, after pulverizing, wind send, carry out yellow after cooling and the weighing;

(b) behind the continuous-dissolution, behind temperature adjustment, pre-deaeration, carry out I road KKF and filter;

(c) carrying out the II road behind temperature adjustment, the rapidly defoaming filters;

(d) fine hair moulding after spinning, drawing-off, the cut-out;

(e) disacidify washing, desulfurization, washing, bleaching;

(f) wash, oil, wet shredding, wind get product after sending, packing.

8. the preparation technology of fibroin blending regeneration cellulose fiber according to claim 7 is characterized in that:

The workflow at alkali station is: liquid caustic soda carries out yellow through new liquid allotment post precipitation; Wherein, a solid caustic soda dissolving back part enters new liquid allotment precipitation, and another part is the concentrated base precipitation; New liquid allotment precipitation gets pressed liquor behind dipping, more after filtering, flood allotment.

9. the preparation technology of fibroin blending regeneration cellulose fiber according to claim 7 is characterized in that:

The workflow at acid station is: spinning is reclaimed and enter tempering tank behind prefiltration, enters kerve and circulating pump more respectively; Behind graphite heater, head tank, enter spinning machine successively behind the quartz sand filtration.

10. the preparation-obtained fibroin blending regeneration cellulose fiber of the preparation technology of the described fibroin blending regeneration cellulose fiber of claim 1.

Images