CN108676110A - A kind of method of MMA monomer castings polymerization production organic glass - Google Patents
A kind of method of MMA monomer castings polymerization production organic glass Download PDFInfo
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- CN108676110A CN108676110A CN201810504852.2A CN201810504852A CN108676110A CN 108676110 A CN108676110 A CN 108676110A CN 201810504852 A CN201810504852 A CN 201810504852A CN 108676110 A CN108676110 A CN 108676110A
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- organic glass
- polymerization
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- mma monomer
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F120/00—Homopolymers 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
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F120/10—Esters
- C08F120/12—Esters of monohydric alcohols or phenols
- C08F120/14—Methyl esters, e.g. methyl (meth)acrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/02—Polymerisation in bulk
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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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)
- Moulds For Moulding Plastics Or The Like (AREA)
- Casting Or Compression Moulding Of Plastics Or The Like (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The present invention relates to a kind of methods that MMA monomer castings polymerization produces organic glass, this method mainly comprises the following steps pre-polymerization processing, moulding, bulk polymerization, die sinking, post-processing, wherein in-lubricant of the highly-efficient lubricant system as entire reaction system is added in pre-polymerization processing, itself has low-down viscosity, the mobility of entire reaction system can be improved simultaneously, gel effect and implode can be effectively avoided, production difficulty is reduced, improves the performance of organic glass.
Description
Technical field
The present invention relates to a kind of production methods of organic glass more particularly to a kind of production of MMA monomer castings polymerization to have
The method of machine glass.
Background technology
Organic glass is widely used, and is not only used in business, light industry, building, chemical industry etc., and advertising decoration,
Using very extensive on sand table model, such as label, billboard, the panel etc. of lamp box.Organic glass is by methyl methacrylate
（MMA）The high-molecular compound being polymerized is a kind of exploitation important thermoplastic earlier, and organic glass has preferable
The advantages that transparency, chemical stability, mechanical property, weatherability, easy dyeing, easy processing and attractive appearance.
Traditional organic glass generally use MMA monomer casting polymerizations production, main raw material(s) includes major ingredient methyl
Methyl acrylate and initiator, effect of initiator during monomer polymerization are particularly important.Its process first has to prepare pre-polymerization
Slurry, and since thermal discharge is big in pre-polymerization slurry process, reaction heat extraction is difficult, will produce auto-acceleration effect, so on the one hand
Hot-spot can be caused and generate implode phenomenon, the viscosity that can also increase pre-polymerization slurry generates gel effect.And current production process
Middle single use initiator azo-bis-isobutyl cyanide is difficult to avoid above-mentioned phenomenon.
Invention content
The present invention is in view of the deficienciess of the prior art, provide a kind of MMA monomer castings polymerization production organic glass
Method, specific technical solution is as follows：
A kind of method of MMA monomer castings polymerization production organic glass, includes the following steps：
Step 1: pre-polymerization is handled
Methyl methacrylate is added in a stirring kettle, injects highly-efficient lubricant system while agitating, stirring is fully backward
Initiator is added in mixed system, stirred tank is warming up to 85 DEG C and stops heating, and maintains stirred tank temperature at 95 DEG C later, waits stirring
It mixes system viscosity in kettle and reaches 1900 ~ 2100cP, cooling is spare；
Step 2: moulding
Moulding is carried out in organic glass particular manufacturing craft after above-mentioned reaction system is filtered, the moulding concrete operations are, by rule
Determine thickness and pad the rubber filler strip that a upper circle is surrounded by glassine paper between the silica glass tablet of two pieces of cleaning, dryings, is clipped with fixture,
Cast, exhaust bubble, sealing；
Step 3: bulk polymerization
The mold of casting complete is hung in constant temperature water tank and is totally submerged, control temperature is at 58 ~ 75 DEG C and keeps 2 ~ 4h；Then it hangs
Go out mold and be put into high temperature drying chamber, control temperature is at 100 ~ 110 DEG C and keeps 2 ~ 6h；
Step 4: die sinking
The mold that polymerization is completed is placed under light protected environment and is cooled to room temperature die sinking；
Step 5: post-processing
Methacrylate sheet intermediate after molding is taken out, trimming is cut, and is packed.
Further, the methyl methacrylate in the step 1, highly-efficient lubricant system and initiator mass parts
Number ratio=（70~73）:（3~5）:（0.2~0.25）.
Further, the highly-efficient lubricant system preparation method in the step 1 is, by ten dihydroxystearic acids, tristearin
Acid and ethyl alcohol are heated to molten condition, then sequentially add fatty alcohol, Sodium Polyacrylate and silicone emulsion, stop antipyretic and stir
To room temperature, adds sodium hydroxide and stir 34 ~ 45min up to the highly-efficient lubricant system.
Further, ten dihydroxystearic acids, stearic acid, ethyl alcohol, fatty alcohol, polypropylene in the highly-efficient lubricant system
Sour sodium, silicone emulsion, sodium hydroxide quality parts ratio=（20~55）:（0.5~3）:（30~60）:（3~5）:（0.3~3）:
（0.05~0.2）:（1~3）
Further, the temperature of the constant temperature water tank in the step 3 is 65 ~ 70 DEG C, and the time is 2.5 ~ 3h.
Further, the temperature of the high temperature drying chamber in the step 3 is 103 ~ 108 DEG C, and the time is 3 ~ 4h.
Beneficial effects of the present invention：The highly-efficient lubricant system added in MMA monomer casting methods can significantly improve at pre-polymerization
The mobility for managing the mixed system in step can effectively avoid gel effect and implode, reduce production difficulty, improve organic glass
Performance.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Embodiment 1
Ten dihydroxystearic acids of 20kg, 0.5kg stearic acid and 30kg ethyl alcohol are heated to molten condition, then sequentially add 3kg
Fatty alcohol, 0.3kg Sodium Polyacrylates and 0.05kg silicone emulsions stop antipyretic and stir to room temperature, add 1kg sodium hydroxides
34 ~ 45min is stirred up to the highly-efficient lubricant system.
70kg methyl methacrylates are added in a stirring kettle, injects 3kg highly-efficient lubricant systems while agitating, stirs
It mixes in fully backward mixed system and 0.2kg azo-bis-isobutyl cyanides is added, stirred tank is warming up to 85 DEG C and stops heating, maintains later
Stirred tank temperature system viscosity in 95 DEG C, kettle to be mixed reaches 1900 ~ 2100cP, and cooling is spare；After reaction system is filtered
Moulding is carried out in organic glass particular manufacturing craft, the moulding concrete operations are the silicon glass in two pieces of cleaning, dryings by specific thickness
The rubber filler strip that a upper circle is surrounded by glassine paper is padded between glass tablet, is clipped, is poured into a mould with fixture, exhaust bubble, sealing；By casting complete
Mold hang in constant temperature water tank and be totally submerged, control temperature at 65 DEG C and keeps 3h；Then it hangs out mold and is put into high temperature drying chamber,
Control temperature at 103 DEG C and keeps 4h；The mold that polymerization is completed is placed under light protected environment and is cooled to room temperature die sinking；Taking-up is opened
Intermediate methacrylate sheet, trimming are cut after mould, are packed.
The MMA monomer casting polymerizations produce the obtained highly-efficient lubricant system in the pre-polymerization processing of organic glass method
Solid content is 30%, and average grain diameter is 30 μm, viscosity 400mPaS, highly-efficient lubricant system conduct in the pre-polymerization processing step
In-lubricant makes the mobility of entire reaction system that in-lubricant raising 15% relatively be not used.
Embodiment 2
Ten dihydroxystearic acids of 22.5kg, 1.5kg stearic acid and 45kg ethyl alcohol are heated to molten condition, then sequentially added
4kg fatty alcohols, 1.5kg Sodium Polyacrylates and 0.15kg silicone emulsions stop antipyretic and stir to room temperature, add 2kg hydrogen-oxygens
Change sodium and stirs 34 ~ 45min up to the highly-efficient lubricant system.
72kg methyl methacrylates are added in a stirring kettle, injects 4kg highly-efficient lubricant systems while agitating, stirs
It mixes in fully backward mixed system and 0.23kg azo-bis-isobutyl cyanides is added, stirred tank is warming up to 85 DEG C and stops heating, Zhi Houwei
It holds stirred tank temperature system viscosity in 95 DEG C, kettle to be mixed and reaches 1900 ~ 2100cP, cooling is spare；Reaction system is filtered
Moulding is carried out in organic glass particular manufacturing craft afterwards, the moulding concrete operations are the silicon in two pieces of cleaning, dryings by specific thickness
The rubber filler strip that a upper circle is surrounded by glassine paper is padded between glass plate, is clipped, is poured into a mould with fixture, exhaust bubble, sealing；It will pour
At mold hang in constant temperature water tank and be totally submerged, control temperature at 68 DEG C and keeps 2.8h；Then it hangs out mold and is put into high temperature
Drying chamber, control temperature at 1.5 DEG C and keep 3.5h；The mold that polymerization is completed is placed under light protected environment and is cooled to room temperature out
Mould；Methacrylate sheet intermediate after molding is taken out, trimming is cut, and is packed.
The MMA monomer casting polymerizations produce the obtained highly-efficient lubricant system in the pre-polymerization processing of organic glass method
Solid content is 25%, and average grain diameter is 28 μm, viscosity 300mPaS, highly-efficient lubricant system conduct in the pre-polymerization processing step
In-lubricant makes the mobility of entire reaction system that in-lubricant raising 18% relatively be not used.
Embodiment 3
Ten dihydroxystearic acids of 25kg, 3kg stearic acid and 60kg ethyl alcohol are heated to molten condition, then sequentially add 5kg fat
Fat alcohol, 3kg Sodium Polyacrylates and 0.2kg silicone emulsions stop antipyretic and stir to room temperature, add the stirring of 3kg sodium hydroxides
34 ~ 45min is up to the highly-efficient lubricant system.
73kg methyl methacrylates are added in a stirring kettle, injects 5kg highly-efficient lubricant systems while agitating, stirs
It mixes in fully backward mixed system and 0.25kg azo-bis-isobutyl cyanides is added, stirred tank is warming up to 85 DEG C and stops heating, Zhi Houwei
It holds stirred tank temperature system viscosity in 95 DEG C, kettle to be mixed and reaches 1900 ~ 2100cP, cooling is spare；Reaction system is filtered
Moulding is carried out in organic glass particular manufacturing craft afterwards, the moulding concrete operations are the silicon in two pieces of cleaning, dryings by specific thickness
The rubber filler strip that a upper circle is surrounded by glassine paper is padded between glass plate, is clipped, is poured into a mould with fixture, exhaust bubble, sealing；It will pour
At mold hang in constant temperature water tank and be totally submerged, control temperature at 70 DEG C and keeps 2.5h；Then it hangs out mold and is put into high temperature
Drying chamber, control temperature at 108 DEG C and keep 3h；The mold that polymerization is completed is placed under light protected environment and is cooled to room temperature die sinking；
Methacrylate sheet intermediate after molding is taken out, trimming is cut, and is packed.
The MMA monomer casting polymerizations produce the obtained highly-efficient lubricant system in the pre-polymerization processing of organic glass method
Solid content is 33%, and average grain diameter is 35 μm, viscosity 500mPaS, highly-efficient lubricant system conduct in the pre-polymerization processing step
In-lubricant makes the mobility of entire reaction system that in-lubricant raising 12% relatively be not used.
The spy that ten dihydroxystearic acids easily solidify after there is high temperature melt to cool down again in the highly-efficient lubricant system of this method
Property, therefore thin film is easily generated on organic glass surface, the auxiliary agent being dispersed therein also equably is covered in organic glass table
Face, and highly-efficient lubricant system serves not only as in-lubricant and is present in organic glass kind, while still releasing agent, it is convenient subsequently to open
The separation of organic glass and mold in mould step.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.
Claims (6)
1. a kind of method of MMA monomer castings polymerization production organic glass, includes the following steps：
Step 1: pre-polymerization is handled
Methyl methacrylate is added in a stirring kettle, injects highly-efficient lubricant system while agitating, stirring is fully backward
Initiator is added in mixed system, stirred tank is warming up to 85 DEG C and stops heating, and maintains stirred tank temperature at 95 DEG C later, waits stirring
It mixes system viscosity in kettle and reaches 1900 ~ 2100cP, cooling is spare；
Step 2: moulding
Moulding is carried out in organic glass particular manufacturing craft after above-mentioned reaction system is filtered, the moulding concrete operations are, by rule
Determine thickness and pad the rubber filler strip that a upper circle is surrounded by glassine paper between the silica glass tablet of two pieces of cleaning, dryings, is clipped with fixture,
Cast, exhaust bubble, sealing；
Step 3: bulk polymerization
The mold of casting complete is hung in constant temperature water tank and is totally submerged, control temperature is at 58 ~ 75 DEG C and keeps 2 ~ 4h；Then it hangs
Go out mold and be put into high temperature drying chamber, control temperature is at 100 ~ 110 DEG C and keeps 2 ~ 6h；
Step 4: die sinking
The mold that polymerization is completed is placed under light protected environment and is cooled to room temperature die sinking；
Step 5: post-processing
Methacrylate sheet intermediate after molding is taken out, trimming is cut, and is packed.
2. a kind of method of MMA monomer castings polymerization production organic glass as described in claim 1, which is characterized in that institute
State the quality parts ratio of methyl methacrylate in step 1, highly-efficient lubricant system and initiator=（70~73）:（3~5）:
（0.2~0.25）.
3. a kind of method of MMA monomer castings polymerization production organic glass as described in claim 1, which is characterized in that institute
It is to be heated to melting by ten dihydroxystearic acids, stearic acid and ethyl alcohol to state the highly-efficient lubricant system preparation method in step 1
Then state sequentially adds fatty alcohol, Sodium Polyacrylate and silicone emulsion, stop antipyretic and stir to room temperature, add hydrogen-oxygen
Change sodium and stirs 34 ~ 45min up to the highly-efficient lubricant system.
4. a kind of method of MMA monomer castings polymerization production organic glass as claimed in claim 2, which is characterized in that institute
State ten dihydroxystearic acids, stearic acid, ethyl alcohol, fatty alcohol, Sodium Polyacrylate, silicone emulsion, hydrogen-oxygen in highly-efficient lubricant system
The quality parts ratio of change sodium=（20~55）:（0.5~3）:（30~60）:（3~5）:（0.3~3）:（0.05~0.2）:（1~3）.
5. a kind of method of MMA monomer castings polymerization production organic glass as described in claim 1, which is characterized in that institute
The temperature for stating the constant temperature water tank in step 3 is 65 ~ 70 DEG C, and the time is 2.5 ~ 3h.
6. a kind of method of MMA monomer castings polymerization production organic glass as described in claim 1, which is characterized in that institute
The temperature for stating the high temperature drying chamber in step 3 is 103 ~ 108 DEG C, and the time is 3 ~ 4h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810504852.2A CN108676110A (en) | 2018-05-24 | 2018-05-24 | A kind of method of MMA monomer castings polymerization production organic glass |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810504852.2A CN108676110A (en) | 2018-05-24 | 2018-05-24 | A kind of method of MMA monomer castings polymerization production organic glass |
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| CN108676110A true CN108676110A (en) | 2018-10-19 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110760023A (en) * | 2019-11-13 | 2020-02-07 | 江苏铁锚玻璃股份有限公司 | Formula and synthesis method of large-thickness polymethyl methacrylate plate |
| CN112521559A (en) * | 2020-12-11 | 2021-03-19 | 锦西化工研究院有限公司 | Method for preparing alkyd organic glass plate and alkyd organic glass plate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN88100180A (en) * | 1988-01-20 | 1988-08-03 | 北京市有机玻璃制品厂 | X-ray-preventing ultraviolet ray synthetic glass and method for making |
| 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 |
| CN103923733B (en) * | 2014-04-30 | 2017-03-29 | 洛阳惠尔纳米科技有限公司 | A kind of water-based lubricant based on ten dihydroxystearic acids and preparation method thereof |
-
2018
- 2018-05-24 CN CN201810504852.2A patent/CN108676110A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN88100180A (en) * | 1988-01-20 | 1988-08-03 | 北京市有机玻璃制品厂 | X-ray-preventing ultraviolet ray synthetic glass and method for making |
| CN103923733B (en) * | 2014-04-30 | 2017-03-29 | 洛阳惠尔纳米科技有限公司 | A kind of water-based lubricant based on ten dihydroxystearic acids and preparation method thereof |
| 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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110760023A (en) * | 2019-11-13 | 2020-02-07 | 江苏铁锚玻璃股份有限公司 | Formula and synthesis method of large-thickness polymethyl methacrylate plate |
| CN112521559A (en) * | 2020-12-11 | 2021-03-19 | 锦西化工研究院有限公司 | Method for preparing alkyd organic glass plate and alkyd organic glass plate |
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Application publication date: 20181019 |