Background technology
Polyvinyl chloride（PVC）Paste resin is as its name suggests that this kind of resin is mainly applied with being made paste forms, Ren MenchangIt is referred to as plasticized paste with this kind of paste（PVC paste）, it is a kind of unique liquid form of the igelite under rough.Paste treeFat is often obtained by emulsion and microsuspending method.
In heating process, molecular thermalmotion aggravation, plasticizer diffuses more readily into the swelling tree in resin particle inside to PVC pasteFat, reduces free plasticizer relative amount, so that PVC paste loses flowability, plasticized paste is in mechanical strength close to " zero "Dry state, this process is referred to as gelation.
PVC gel process is significant in the production of PVC paste product process, for example, dipping in modeling glove productionIn, glove mould after heating is immersed into prefabricated PVC plasticized pastes, the PVC paste near mould forms gel layer, and unnecessary thickener existsBreak away from moulds under Action of Gravity Field, gel layer is plastified and cooled through high temperature and can be made into paste resin gloves.Rubbing method flooring laminate,In the production processes such as support methods artificial leather, slush moulding footwear, also will be by gelation operation.Therefore PVC paste gelatinization performance is to pastingProduct technique and product quality have important influence.
Gelation method of testing mainly has：
1st, Brabender plasticizing instrument method
PVC paste torque variation with temperature is determined under the conditions of constant heatingrate and draw the temperature-torque curve of gelation process.As temperature rises, the temperature that PVC paste sample occurs torque rising is the sample gelling temperature.
2nd, rotation viscometer method
Under a steady temperature, gelation is changed with time and drawn using viscosity in different rotor measure different rangeThe when m- viscograph of journey.For ease of the gelatinization performance of relatively more different system pastes, taken when paste viscosity is reached a certain valueBetween be defined as gelation time, and with the quantitatively characterizing as PVC paste gelatinization performance.
Brabender curve, because programming rate is slower in experiment, the gelation process in test is not equivalent to realityGelation process in production, but Brabender plasticizing instrument can determine overall process of the PVC paste from gelation to fusion plastification, energyEnough gelation features for more fully reflecting PVC paste；The range of viscosities of rotary viscosity design determining is narrower, can only determine relatively low gelThe indicatrix of change degree, and gelation overall process can not be reflected.
The content of the invention
Goal of the invention of the invention is to provide a kind of test accurately, the PVC paste resin gel test of simple structureDevice and method of testing.
Test device of the present invention proposes to adopt the following technical scheme that：
A kind of PVC paste resin gel test device, including heater block, control unit and test groove structure, control unitPart is connected with heater block circuit, and the heating source in heater block uses electronics universal furnace, and electronics universal furnace top is equipped with heatingCopper coin structure, test groove is provided with heating copper coin.
Compared with prior art, simple structure is easy to operation, test result accuracy rate to the present invention of above-mentioned technical proposalIt is high.
Preferred scheme of the invention is：
Control unit includes timer and electric energy-saving temperature controller, and timer and temperature controller are placed in same casing.
The hardened structure of Heated Copper is identical with electronics universal furnace heating surface (area) (HS, 10~20mm of thickness, test groove diameter ∮ 20~50Mm, the mm of depth 3~5.
The technical scheme of method of testing is：
Method of testing, is carried out as follows：
Plasticizer and PVC paste resin are prepared into plasticized paste through Hobart's mixer, plasticized paste is quantitatively adding gelation testIn instrument groove, gelation time is tested at a temperature of 50 DEG C~150 DEG C.
The method of testing, can be visual, and it is wide to determine range of viscosities.
The preferred scheme of method of testing is：
Plasticizer is matched with PVC paste resin by following weight portion：Plasticizer accounts for the 50 of PVC paste resin weight~100%.
Plasticizer is selected from dibutyl phthalate, BBP(Butyl Benzyl Phthalate, dioctyl phthalate, terephthaldehydeOne of dioctyl phthalate, diisononyl phthalate, diisooctyl phthalate or di-n-octyl sebacate.
PVC paste resin is that any commercial grades paste resin.
By plasticizer and PVC paste resin at normal temperatures through N50 Hobarts agitator " 1 " shelves（136 rpm）Stirring 1~5min, " 2 " shelves（281rpm）10~20min of stirring prepares gelation plasticized paste, 12~48h of vacuum defoamation under plasticized paste normal temperatureIt is standby.
Gelation time is tested at 50 DEG C~150 DEG C, 30~50mg vacuum defoamation post-plasticization pastes are added with sample spoonIn copper coin groove and start timing, do not stop stirring with glass bar, stir upward wire drawing on one side, stirring is with per minute 30~50Circle is preferred, and is drawn a circle clockwise or counterclockwise during stirring, and plasticized paste will be stirred to, and stir, to plasticized paste just no longerAdherent glass rod, is gelation terminal.
Specific embodiment
Below in conjunction with the accompanying drawings and embodiment describe in detail the present invention：
A kind of PVC paste resin gel test device, referring to accompanying drawing 1, in figure：Casing 1, connecting wire 2, electronics universal furnace3rd, the hardened structure 4 of Heated Copper, test groove 5.
In the present embodiment, control unit is connected with heater block circuit, and the heating source in heater block is using DL-1 types electricitySub- universal furnace 3, the top of electronics universal furnace 3 is equipped with the hardened structure 4 of Heated Copper, and test groove 5 is provided with the hardened structure 4 of Heated Copper.
Control unit is made up of UP8T types timer and ZNHW type electric energy-saving temperature controllers, timer and temperature controlDevice is placed in same casing.
The heating surface (area) (HS of electronics universal furnace 3 be more than 100 × 100 mm, 0 to 550 DEG C of temperature regulating range, temperature fluctuation is notMore than 0.2 degree, furnace insulation works well.
The hardened structure 4 of Heated Copper is identical with the heating surface (area) (HS of electronics universal furnace 3, thickness 20mm, the mm of test groove diameter ∮ 50,The mm of depth 5.Temperature transducer will be close to hotplate surface and in copper coin test groove 5 structure bottom center.Time set0~0.999.9S of temperature range, precision 0.1S.
The specific embodiment one of method：
Weigh 100g SY-Z170 proper tree cosmetics（Tangshan Alkaili Chloride Co., Ltd.'s product, market can also buy）,80g DOP（Dioctyl phthalate）After mixing, 2min is stirred through N50 Hobarts agitator " 1 " shelves under normal temperature, " 2 " shelves are stirredMix 20min and prepare gelation plasticized paste, through vacuum defoamation device deaeration 12h to bubble-free in plasticized paste, vacuum under plasticized paste normal temperatureDegree 0.1Mpa.Gelation tester timer is zeroed, and sets 102 DEG C of test temperature, the stabilization 45min after temperature reaches, willSY-Z170 resin dedicated plasticized paste samples spoon is added in copper coin groove and starts timing after 30mg vacuum defoamations, uses glass barDo not stop stirring, stir while hot candied upwards, stirring is preferred with per minute 30 circles, is drawn a circle clockwise during stirring, and plasticized paste is allIt is stirred to, and stirs, stirring rod is not just adhered to plasticized paste, is gelation terminal.
Its gelation time is 145s.
Example 2：
Weigh 100g SY-Z140 proper tree cosmetics（Tangshan Alkaili Chloride Co., Ltd.'s product, market can also buy）,After 80g DOP mixing, 2min is stirred through N50 Hobarts agitator " 1 " shelves under normal temperature, " 2 " shelves stirring 20min prepares gelation and increasesModeling paste, through vacuum defoamation device deaeration 12h to bubble-free in plasticized paste, vacuum 0.1Mpa under plasticized paste normal temperature.Gelation is testedInstrument timer is zeroed, and sets 102 DEG C of test temperature, the stabilization 45min after temperature reaches, by SY-Z140 after 30mg vacuum defoamationsResin dedicated plasticized paste sample spoon is added in copper coin groove and starts timing, does not stop stirring with glass bar, stir whileHot candied upwards, stirring is preferred with 30-35 per minute circles, is drawn a circle clockwise during stirring, and plasticized paste will be stirred to, and stirs equalIt is even, stirring rod is not just adhered to plasticized paste, it is gelation terminal.
Its gelation time is 102s.
Example 3：
Weigh 100g SY-Z100 proper tree cosmetics（Tangshan Alkaili Chloride Co., Ltd.'s product, market can also buy）,After 80g DOP mixing, 2min is stirred through N50 Hobarts agitator " 1 " shelves under normal temperature, " 2 " shelves stirring 20min prepares gelation and increasesModeling paste, through vacuum defoamation device deaeration 12h to bubble-free in plasticized paste, vacuum 0.1Mpa under plasticized paste normal temperature.Gelation is testedInstrument timer is zeroed, and sets 102 DEG C of test temperature, the stabilization 45min after temperature reaches, by SY-Z100 after 30mg vacuum defoamationsResin dedicated plasticized paste sample spoon is added in copper coin groove and starts timing, does not stop stirring with glass bar, stir whileHot candied upwards, stirring is preferred with 30-35 per minute circles, is drawn a circle clockwise during stirring, and plasticized paste will be stirred to, and stirs equalIt is even, stirring rod is not just adhered to plasticized paste, it is gelation terminal.
Its gelation time is 61s.
Example 4：
Weigh 100g SY-Z170（Tangshan Alkaili Chloride Co., Ltd.'s product, market can also buy）Proper tree cosmetics,80g DOTP（DOTP）After mixing, 2min is stirred through N50 Hobarts agitator " 1 " shelves under normal temperature, " 2 " shelves are stirredMix 20min and prepare gelation plasticized paste, through vacuum defoamation device deaeration 12h to bubble-free in plasticized paste, vacuum under plasticized paste normal temperatureDegree 0.1Mpa.Gelation tester timer is zeroed, and sets 102 DEG C of test temperature, the stabilization 45min after temperature reaches, willSY-Z170 resin dedicated plasticized paste samples spoon is added in copper coin groove and starts timing after 30mg vacuum defoamations, uses glass barDo not stop stirring, stir while hot candied upwards, stirring is preferred with 30-35 per minute circles, is drawn a circle clockwise during stirring, is plasticizedPaste will be stirred to, and stir, and stirring rod is not just adhered to plasticized paste, be gelation terminal.
Its gelation time is 158s.
Example 5
Weigh 100g SY-Z170 proper tree cosmetics, 80g ATBC（The positive definite ester of acetyl tributyl citrate three）After mixing, through N50 under normal temperatureHobart's agitator " 1 " shelves stir 2min, and " 2 " shelves stirring 20min prepares gelation plasticized paste, de- through vacuum under plasticized paste normal temperatureBubbler deaeration 12h is to bubble-free in plasticized paste, vacuum 0.1Mpa.Gelation tester timer is zeroed, and sets test temperature102 DEG C, the stabilization 45min after temperature reaches adds the resin dedicated plasticized pastes of SY-Z170 after 30mg vacuum defoamations with sample spoonIn copper coin groove and start timing, do not stop stirring with glass bar, stir upward wire drawing on one side, stirring is with 30-35 per minuteCircle is preferred, and is drawn a circle clockwise during stirring, and plasticized paste will be stirred to, and stir, and stirring is not just adhered to plasticized pasteRod, is gelation terminal.
Its gelation time is 327s.
Example 6
Weigh 100g SY-Z170 proper tree cosmetics, 80g DINCH（Hexamethylene 1,2- dioctyl phthalate diisononyl esters）After mixing, often2min is stirred through N50 Hobarts agitator " 1 " shelves under temperature, " 2 " shelves stirring 20min prepares gelation plasticized paste, plasticized paste normal temperatureIt is lower through vacuum defoamation device deaeration 12h to bubble-free in plasticized paste, vacuum 0.1Mpa.Gelation tester timer is zeroed, ifDetermine 102 DEG C of test temperature, the stabilization 45min after temperature reaches uses the resin dedicated plasticized pastes of SY-Z170 after 30mg vacuum defoamationsSample spoon is added in copper coin groove and starts timing, does not stop stirring with glass bar, stir upward wire drawing on one side, and stirring is with everyMinute 30-35 circle is preferred, and is drawn a circle clockwise during stirring, and plasticized paste will be stirred to, and stir, to plasticized paste just notAdhesion stirring rod, is gelation terminal.
Its gelation time is 176s.
Six examples more than, it can be seen that the parameter such as gelation time and resin polymerization degree, temperature is related, with downstream plusResult is identical in work production process.The gelation process in actual production can be simulated using this kind of method, so as to instruct downstreamProcessing, while provide data for naval stores is modified supporting.