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CN107793508A - A kind of preparation method of lucite - Google Patents

A kind of preparation method of lucite Download PDF

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Publication number
CN107793508A
CN107793508A CN201711102648.XA CN201711102648A CN107793508A CN 107793508 A CN107793508 A CN 107793508A CN 201711102648 A CN201711102648 A CN 201711102648A CN 107793508 A CN107793508 A CN 107793508A
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CN
China
Prior art keywords
polymerization
lucite
high temperature
temperature
azodiisobutyronitrile
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201711102648.XA
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Chinese (zh)
Inventor
周小二
王可
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Anhui Xintao Optoelectronics Technology Co Ltd
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Anhui Xintao Optoelectronics Technology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Anhui Xintao Optoelectronics Technology Co Ltd filed Critical Anhui Xintao Optoelectronics Technology Co Ltd
Priority to CN201711102648.XA priority Critical patent/CN107793508A/en
Publication of CN107793508A publication Critical patent/CN107793508A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F120/00Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
    • C08F120/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F120/10Esters
    • C08F120/12Esters of monohydric alcohols or phenols
    • C08F120/14Methyl esters, e.g. methyl (meth)acrylate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F4/00Polymerisation catalysts
    • C08F4/04Azo-compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L33/00Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
    • C08L33/04Homopolymers or copolymers of esters
    • C08L33/06Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
    • C08L33/10Homopolymers or copolymers of methacrylic acid esters
    • C08L33/12Homopolymers or copolymers of methyl methacrylate

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

The present invention relates to the technology for producing field of lucite, the improvement of pre-polymerization paste composition in the preparation process of lucite is related particularly to, this method mainly comprises the following steps pre-polymerization slurry and prepare-fills mould-low temperature polymerization-high temperature polymerization-cooling demoulding-adsorbing separation;Wherein using ABVN and the composite initiator system of azodiisobutyronitrile during prepared by pre-polymerization slurry.Beneficial effects of the present invention are:The use range of initiator is widened, it is gone for the pre- collecting process of a variety of thermal cracking monomers;The characteristics of decomposition rate is fast at high temperature using medium temperature initiator, the azodiisobutyronitrile of surplus is set quickly to consume in a short time;So as to both ensure that viscosity reaches production requirement in pre-polymerization slurry preparation process, reduce the residual of initiator again, shorten the pre-polymerization time, eliminate the probability that implode occurs for low temperature polymerization stage;Lucite production process disclosed by the invention is stable, and product performance index reaches industry standard.

Description

A kind of preparation method of lucite
Technical field
The present invention relates to the technology for producing field of lucite, in the preparation process for relating particularly to lucite The improvement of pre-polymerization paste composition.
Background technology
Lucite is the high-molecular compound formed by methyl methacrylate polymerization, is that a kind of exploitation is important earlier Thermoplastic, lucite have the preferably transparency, chemical stability, mechanical property and weatherability, easy dyeing, Yi Jia Work, the advantages that attractive appearance.
Lucite is widely used, and lucite is not only used in business, light industry, building, chemical industry etc..It is and organic Glass is produced on advertising decoration, on sand table model using quite varied, such as:Label, billboard, panel of lamp box etc..
The preparation method of lucite have it is a variety of, such as mounting method, pressure sintering, inlaying process, Vertical Mill method, disconnected mill method and fire bending Method, above method can be used alternatingly in practical operation, and traditional lucite preparation method mainly uses pressure sintering, prepare During first have to carry out the preparation of pre-polymerization slurry, initiator plays an important role herein, is prepared in traditional lucite During compared with frequently with a kind of initiator be ABVN, because its activity is big, efficiency of initiation is high and enjoys favor.
Occurs the Time Inconsistency of gel phenomenon during pre-polymerization material, some is after traditional pre-polymerization material step Viscosity can not reach technique requirement cause after the step of can not be smoothed out, in order that viscosity can reach requirement, mainly The method of use is to increase the dosage of initiator ABVN, but the dosage of excessively increase initiator can then cause low temperature There is implode phenomenon in polymerization stage, and the performance for the lucite produced is unstable, and the usage amount of initiator is big, during pre-polymerization Between also grow.
The content of the invention
It is an object of the invention to provide a kind of preparation method of lucite, and preparing lucite using this kind of method can With change in pre-polymerization slurry process is prepared part pulp gel phenomenon be in the presence of it is later, while and can elimination low temperature gather The implode phenomenon in conjunction stage, stable processing technique, properties of product reach defined standard.
In order to achieve the above object, the present invention is achieved by the following technical solutions:A kind of preparation side of lucite Method, mainly include the following steps that:
(1)It is prepared by pre-polymerization slurry:Major ingredient methyl methacrylate is injected in heating kettle, is stirred in addition, in whipping process The middle composite initiator system for adding ABVN and azodiisobutyronitrile, 80 DEG C of insulation 20min are heated to, are heated afterwards To 100 DEG C, boiling 20-30 min are kept, after determining that material viscosities reach 40-60s using -4 glasss of measurements of painting, cooling is standby;
(2)Fill mould:The middle product obtained through above-mentioned steps carry out filling mould in lucite particular manufacturing craft after filtering, fill mould mistake Cheng Caiyong acrylic boards sizing device for exerting ensures that sheet metal thickness is uniform;
(3)Low temperature polymerization:The mould completed through filling mould is placed in cage car, is transferred cage car to 45-65 DEG C of perseverance by row loop wheel machine structure It is totally submerged in heated pool, Immersion time 3-6 h, and carries out low temperature polymerization;
(4)High temperature polymerization:After the completion of above-mentioned steps low temperature polymerization, hung out through cage car from pond, be pushed into 105-120 DEG C of high temperature Stove high temperature polymerization 2-10 h;
(5)Cool demoulding:After the completion of above-mentioned steps high temperature polymerization, by cage car by being released in drying room, the room of spacious lucifuge is placed in In warm environment, molded after temperature is down to room temperature;
(6)Adsorbing separation:After the completion of demoulding, the adsorbent equipment made by acrylic board is separated into template and mould, removes into Pack, be put in storage after template.
The step(1)The molar ratio of middle ABVN and azodiisobutyronitrile is 1:0.4-0.7.
As a kind of preferred embodiment of the present invention, the step(1)Middle ABVN and azodiisobutyronitrile Molar ratio be 1:0.58-0.63
As a kind of preferred embodiment of the present invention, the step(3)Temperature in middle constant temperature pool is 47-53 DEG C, submergence Time is 3.5-4h.
As a kind of preferred embodiment of the present invention, the step(4)The temperature of high temperature stove is 108-115 DEG C, instead It is 3-6h between seasonable.
As a kind of preferred embodiment of the present invention, the step(4)The temperature of high temperature stove is 112-114 DEG C, instead It is 2.5-5h between seasonable.
Beneficial effects of the present invention are:The present invention has widened the use range of initiator, goes for a variety of thermal crackings The pre- collecting process of monomer, using medium temperature initiator quick inhibition impurity in consumption system the characteristics of active high at high temperature, The characteristics of decomposition rate is fast under its high temperature is utilized simultaneously, the azodiisobutyronitrile of surplus is quickly consumed in a short time.With The ABVN of ratio of the present invention and the composite initiator system of azodiisobutyronitrile, which feed intake, to be ensured In the case that viscosity reaches production requirement in pre-polymerization slurry preparation process, the residual of initiator in pre-polymerization material is reduced, shortens pre-polymerization Time, the probability that implode phenomenon occurs for low temperature polymerization stage, stable processing technique are eliminated, plate property reaches industry standard.
Embodiment
Structure, principle and the course of work of the present invention are further described with specific embodiment below, but the present invention Protection domain be not limited thereto.
Embodiment 1
A kind of preparation method of lucite, is mainly included the following steps that:
(1)It is prepared by pre-polymerization slurry:Major ingredient methyl methacrylate is injected in heating kettle, is stirred in addition, in whipping process The middle composite initiator system for adding ABVN and azodiisobutyronitrile, 80 DEG C of insulation 20min are heated to, are heated afterwards To 100 DEG C, boiling 20-30 min are kept, after determining that material viscosities reach 40-60 s using -4 glasss of measurements of painting, cooling is standby;
(2)Fill mould:The middle product obtained through above-mentioned steps carry out filling mould in lucite particular manufacturing craft after filtering, fill mould mistake Cheng Caiyong acrylic boards sizing device for exerting ensures that sheet metal thickness is uniform;
(3)Low temperature polymerization:The mould completed through filling mould is placed in cage car, is transferred cage car to 45-65 DEG C of perseverance by Hang Diao mechanisms It is totally submerged in heated pool, Immersion time 3-6 h, and carries out low temperature polymerization;
(4)High temperature polymerization:After the completion of above-mentioned steps low temperature polymerization, hung out through cage car from pond, be pushed into 105-120 DEG C of high temperature Stove high temperature polymerization 2-10 h;
(5)Cool demoulding:After the completion of above-mentioned steps high temperature polymerization, by cage car by being released in drying room, the room of spacious lucifuge is placed in In warm environment, molded after temperature is down to room temperature;
(6)Adsorbing separation:After the completion of demoulding, the adsorbent equipment made by acrylic board is separated into template and mould, removes into Pack, be put in storage after template.
Wherein described step(1)The molar ratio of middle ABVN and azodiisobutyronitrile is 1:0.4-0.7.
It is that inventor develops on the basis of creative work has been carried out that this kind, which triggers agent prescription, two different heptan of azo Nitrile and azodiisobutyronitrile are all azo-initiators, and the activity of ABVN is big, and efficiency of initiation is high, the isobutyl of azo two Nitrile, a kind of free radical is only formed, it is more stable without other side reactions, in process of production such as only addition ABVN The viscosity that words normally result in pre-polymerization slurry can not reach requirement, it is impossible to carry out the production of next step, in that case, mostly The dosage that manufacturer can select to improve ABVN solves the above problems, and improves the dosage of ABVN simply Then it can cause the phenomenon of implode occur during low temperature polymerization again.
And the present invention creatively adds a certain proportion of azodiisobutyronitrile wherein, make ABVN and idol The molar ratio of nitrogen bis-isobutyronitrile is controlled 1:In the range of 0.4-0.7, the formula is effectively using azodiisobutyronitrile low The high activity that just has under temperature and at high temperature fast decoupled produce the performance of a large amount of living radical initiation reactions, make it 80 DEG C insulation 20min, the inhibition impurity in quick consumption system;The characteristics of decomposition rate is fast under its high temperature is utilized simultaneously, short The azodiisobutyronitrile of surplus is set quickly to consume in time;Now later phenomenon can be dissolved with changing section pulp gel, is glued Industry requirement can be reached on degree;A large amount of residuals of initiator in pre-polymerization material are reduced, shortens the time of pre-polymerization, eliminates low temperature and gather The probability of implode phenomenon, stable processing technique occur for the conjunction stage, and the plate property produced reaches industry standard;This kind compound to draw Hair agent system has widened the use range of initiator, is adapted to the pre- collecting process of a variety of thermal cracking monomers.
The step(3)Temperature in middle constant temperature pool is 47-53 DEG C, Immersion time 3.5-4h;Enter under this condition Row low temperature polymerization, by polymerization time control in shorter scope, the efficiency of polymerization is improved, helping, which reduces enterprise, is produced into This.
The step(4)The temperature of high temperature stove is 108-115 DEG C, reaction time 3-6h;Under this condition can be steady Surely the effect of high temperature polymerization is ensured, and can saves the reaction time, improves production efficiency.
Embodiment 2
The difference of embodiment 2 and embodiment 1 is, the step(1)Middle ABVN and azodiisobutyronitrile feed intake Mol ratio is 1:0.58-0.63.
Inventor subsequently compares by repetition test, it is determined that more preferably an ABVN and azodiisobutyronitrile Molar ratio scope, decomposition that can be most fast produces initiation reaction performance after living radical, is further ensured that slurry occurs The time of gel phenomenon.
Embodiment 3
The difference from Example 2 of embodiment 3 is, the step(4)The temperature of high temperature stove is 112-114 DEG C, during reaction Between be 2.5-5h.The reaction of high temperature polymerization step during prepared by lucite can be significantly reduced using this kind of reaction condition Time, shorten the flow time of preparation, hence it is evident that production efficiency is improved, and inventor has found after continuously attempting to, in the temperature model Interior progress high temperature polymerization machine-shaping best results are enclosed, the light transmittance of lucite is high, good mechanical property.
The specific embodiment of the present invention is the foregoing is only, but the technical characteristic of the present invention is not limited thereto, Ren Heben The other embodiment that the technical staff in field draws in the case where not departing from technical scheme all should cover the present invention's Among the scope of the claims.

Claims (5)

1. a kind of preparation method of lucite, it is characterised in that specifically include following steps:
(1)It is prepared by pre-polymerization slurry:Major ingredient methyl methacrylate is injected in heating kettle, is stirred in addition, in whipping process The middle composite initiator system for adding ABVN and azodiisobutyronitrile, 80 DEG C of insulation 20min are heated to, are heated afterwards To 100 DEG C, boiling 20-30 min are kept, after determining that material viscosities reach 40-60 s using -4 glasss of measurements of painting, cooling is standby;
(2)Fill mould:The middle product obtained through above-mentioned steps carry out filling mould in lucite particular manufacturing craft after filtering, fill mould mistake Cheng Caiyong acrylic boards sizing device for exerting ensures that sheet metal thickness is uniform;
(3)Low temperature polymerization:The mould completed through filling mould is placed in cage car, is transferred cage car to 45-65 DEG C of perseverance by row loop wheel machine structure It is totally submerged in heated pool, Immersion time 3-6 h, and carries out low temperature polymerization;
(4)High temperature polymerization:After the completion of above-mentioned steps low temperature polymerization, hung out through cage car from pond, be pushed into 105-120 DEG C of high temperature Stove high temperature polymerization 2-10 h;
(5)Cool demoulding:After the completion of above-mentioned steps high temperature polymerization, by cage car by being released in drying room, the room of spacious lucifuge is placed in In warm environment, molded after temperature is down to room temperature;
(6)Adsorbing separation:After the completion of demoulding, the adsorbent equipment made by acrylic board is separated into template and mould, removes into Pack, be put in storage after template;
The step(1)The molar ratio of middle ABVN and azodiisobutyronitrile is 1:0.4-0.7.
A kind of 2. preparation method of lucite according to claim 1, it is characterised in that the step(1)Middle azo The molar ratio of two different heptonitriles and azodiisobutyronitrile is 1:0.58-0.63.
A kind of 3. preparation method of lucite according to claim 1, it is characterised in that the step(3)Middle constant temperature Temperature in pond is 47-53 DEG C, Immersion time 3.5-4h.
A kind of 4. preparation method of lucite according to claim 1, it is characterised in that the step(4)High temperature The temperature of stove is 108-115 DEG C, reaction time 3-6h.
A kind of 5. preparation method of lucite according to claim 1, it is characterised in that the step(4)High temperature The temperature of stove is 112-114 DEG C, reaction time 2.5-5h.
CN201711102648.XA 2017-11-10 2017-11-10 A kind of preparation method of lucite Pending CN107793508A (en)

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Application Number Priority Date Filing Date Title
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Application Number Priority Date Filing Date Title
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108772997A (en) * 2018-05-24 2018-11-09 安徽新涛光电科技有限公司 A kind of organic glass water-bath maintaining process method
CN109369843A (en) * 2018-11-14 2019-02-22 安徽新涛光电科技有限公司 A kind of preparation process of antistatic organic glass
CN110091452A (en) * 2019-04-24 2019-08-06 惠达卫浴股份有限公司 A kind of production method of one acrylic bathtub
CN110938166A (en) * 2019-12-16 2020-03-31 锦西化工研究院有限公司 Method for preparing composite large-thickness aviation organic glass plate

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102746424A (en) * 2011-04-20 2012-10-24 南京华狮化工有限公司 Free radical polymerization initiator composition and its application
CN105237673A (en) * 2015-10-19 2016-01-13 陕西理工学院 Method for casting PMMA board under room temperature polymerization condition and spraying polymerization device
CN106188408A (en) * 2016-08-05 2016-12-07 安徽新涛光电科技有限公司 High transparent high resiliency lucite and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102746424A (en) * 2011-04-20 2012-10-24 南京华狮化工有限公司 Free radical polymerization initiator composition and its application
CN105237673A (en) * 2015-10-19 2016-01-13 陕西理工学院 Method for casting PMMA board under room temperature polymerization condition and spraying polymerization device
CN106188408A (en) * 2016-08-05 2016-12-07 安徽新涛光电科技有限公司 High transparent high resiliency lucite and preparation method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108772997A (en) * 2018-05-24 2018-11-09 安徽新涛光电科技有限公司 A kind of organic glass water-bath maintaining process method
CN109369843A (en) * 2018-11-14 2019-02-22 安徽新涛光电科技有限公司 A kind of preparation process of antistatic organic glass
CN110091452A (en) * 2019-04-24 2019-08-06 惠达卫浴股份有限公司 A kind of production method of one acrylic bathtub
CN110938166A (en) * 2019-12-16 2020-03-31 锦西化工研究院有限公司 Method for preparing composite large-thickness aviation organic glass plate
CN110938166B (en) * 2019-12-16 2022-04-05 锦西化工研究院有限公司 Method for preparing composite large-thickness aviation organic glass plate

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Application publication date: 20180313

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