CN109280122A - A kind of bubble-free lucite tube and preparation method thereof - Google Patents
A kind of bubble-free lucite tube and preparation method thereof Download PDFInfo
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- CN109280122A CN109280122A CN201810928896.8A CN201810928896A CN109280122A CN 109280122 A CN109280122 A CN 109280122A CN 201810928896 A CN201810928896 A CN 201810928896A CN 109280122 A CN109280122 A CN 109280122A
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- bubble
- free
- lucite tube
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- degrees celsius
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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
- C08F220/00—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 a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions 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
- C08L33/04—Homopolymers or copolymers of esters
- C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
- C08L33/10—Homopolymers or copolymers of methacrylic acid esters
- C08L33/12—Homopolymers or copolymers of methyl methacrylate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/18—Applications used for pipes
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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)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
Disclosed by the invention to belong to organic glass technical field, specially a kind of bubble-free lucite tube and preparation method thereof, which includes following constituent: methyl methacrylate；Initiator；The preparation method of comonomer and modifying agent, the bubble-free lucite tube includes the following steps: S1: feedstock processing；S2: prepolymerization；S3: rear polymerization；S4: moulding by casting；S5: heat treatment；S6: demoulding packaging, a kind of bubble-free lucite tube and preparation method thereof that the invention proposes, polar group is introduced by copolymerization, by being cross-linked to form space network, the glass transition temperature of lucite tube can be effectively improved, and pass through optimization reaction temperature and initiator amount, it enables to lucite tube to reach hardness and maximizes effect, and it can effectively reduce the bubble generated in decomposable process, and the introducing of bubble can be prevented, product light transmittance is improved, the invention preparation method is simple, and defect rate is low.
Description
Technical field
The present invention relates to organic glass technical field, specially a kind of bubble-free lucite tube and preparation method thereof.
Background technique
Organic glass is the high-molecular compound as made of methyl methacrylate polymerization.It is that a kind of exploitation is important earlier
Thermoplastic.Organic glass is divided into colorless and transparent, colored transparent, pearly-lustre, four kinds of organic glass of embossing.Organic glass is commonly called as Asia
Gram force, middle a surname's acryl, sub- Gree, organic glass have the preferable transparency, chemical stability, mechanical property and weatherability,
The advantages that easy dyeing, easy processing, attractive appearance.Lucite tube is widely used in advertising model, craftwork and instrument and meter etc.
Field.Existing lucite tube during production, inside be easy to appear bubble, and structural strength is lower, light transmittance
Difference, glass transition temperature is lower, for this purpose, it is proposed that a kind of bubble-free lucite tube and preparation method thereof.
Summary of the invention
The purpose of the present invention is to provide a kind of bubble-free lucite tubes and preparation method thereof, to solve above-mentioned background skill
The existing lucite tube proposed in art during production, inside be easy to appear bubble, and structural strength is lower, thoroughly
Light rate is poor, the lower problem of glass transition temperature.
To achieve the above object, the invention provides the following technical scheme: a kind of bubble-free lucite tube, the bubble-free have
Machine glass tube includes following constituent:
Methyl methacrylate: 90-110 parts；Initiator: 0.125-0.15 parts；Comonomer: 6-10 parts and modifying agent: 0.2-
0.3 part.
Preferably, the initiator is azodiisobutyronitrile.
Preferably, the comonomer methacrylic acid.
Preferably, the modifying agent includes plasticizer and crosslinking agent.
A kind of preparation method of bubble-free lucite tube, the preparation method of the bubble-free lucite tube include following step
It is rapid:
S1: feedstock processing: cleaning methyl methacrylate, obtains clear methyl methacrylate solution, then does
Dry purifying methyl acrylic methylmethacrylate monomer；
S2: step S1 treated methyl methacrylate list prepolymerization: will be added in initiator, comonomer and modifying agent
Body vibrate in heating, and the viscosity no-load voltage ratio of observation liquid, stops when viscosity is close to silicone oil state during oscillation
Heating oscillation, then uses oil bath heated at constant temperature 18-22 hours；
S3: rear polymerization: after the completion of oil bath, being put into baking oven, and temperature rises to 85-100 degrees Celsius, reacts 20-30 minutes, so that
Complete monomer conversion, rear polymerization are completed；
S4: moulding by casting: taking organic glass pipe mold, and the slurry after polymerization is slowly poured in the inner, and casting height control exists
6-8 centimetres, then it is placed on heating 3-4 hours in 48-54 degrees Celsius of water-bath；
S5: heat treatment: after the completion of water-bath, organic glass pipe mold being placed in baking oven and is heat-treated, heat treatment temperature 86-
96 degrees Celsius, heat treatment time is 1-2 hours；
S6: it demoulding packaging: after the completion of heat treatment, demoulded, polished, polished and is packed.
Preferably, it in the step S1, is cleaned using 10% sodium hydroxide solution and 60% ultrapure water, wash number is
4-5 times.
Preferably, the oil bath heating temperature in the step S2 is 40-45 degrees Celsius.
Preferably, in the step S4, organic glass pipe mold needs to be preheated using baking oven before use, preheating temperature
Degree is 95-105 degrees Celsius.
Compared with prior art, the beneficial effects of the present invention are: a kind of bubble-free lucite tube that the invention proposes and
Preparation method, organic glass can be effectively improved by being cross-linked to form space network by introducing polar group by copolymerization
The glass transition temperature of pipe, and by optimization reaction temperature and initiator amount, enable to lucite tube to reach hardness maximum
Change effect, and can effectively reduce the bubble generated in decomposable process, and the introducing of bubble can be prevented, it is saturating to improve product
Light rate, the invention preparation method is simple, and defect rate is low.
Detailed description of the invention
Fig. 1 is preparation method flow chart of the present invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
The present invention provides a kind of bubble-free lucite tube, which includes following constituent:
Methyl methacrylate: 90-110 parts；Initiator: 0.125-0.15 parts；Comonomer: 6-10 parts and modifying agent: 0.2-
0.3 part, the initiator be azodiisobutyronitrile, the comonomer methacrylic acid, the modifying agent include plasticizer and
Crosslinking agent.
Referring to Fig. 1, the present invention also provides a kind of preparation methods of bubble-free lucite tube:
Embodiment 1
The preparation method of the bubble-free lucite tube includes the following steps:
S1: feedstock processing: cleaning methyl methacrylate, obtains clear methyl methacrylate solution, then does
Dry purifying methyl acrylic methylmethacrylate monomer, is cleaned using 10% sodium hydroxide solution and 60% ultrapure water, wash number 4
It is secondary；
S2: step S1 treated methyl methacrylate list prepolymerization: will be added in initiator, comonomer and modifying agent
Body vibrate in heating, and the viscosity no-load voltage ratio of observation liquid, stops when viscosity is close to silicone oil state during oscillation
Heating oscillation, then uses oil bath heated at constant temperature 18 hours, and oil bath heating temperature is 40 degrees Celsius；
S3: rear polymerization: after the completion of oil bath, being put into baking oven, and temperature rises to 85 degrees Celsius, reacts 20 minutes, so that monomer is complete
Full conversion, rear polymerization are completed；
S4: moulding by casting: taking organic glass pipe mold, and the slurry after polymerization is slowly poured in the inner, and casting height control is 6
Centimetre, be then placed on heating 3 hours in 48 degrees Celsius of water-bath, organic glass pipe mold needed before use using baking oven into
Row preheating, preheating temperature are 95 degrees Celsius；
S5: heat treatment: after the completion of water-bath, organic glass pipe mold being placed in baking oven and is heat-treated, heat treatment temperature 86
Degree Celsius, heat treatment time is 1 hour；
S6: it demoulding packaging: after the completion of heat treatment, demoulded, polished, polished and is packed.
In the present embodiment, methyl methacrylate: 110 parts；Initiator: 0.125 part；Comonomer: 10 parts and modification
Agent: 0.2 part, the initiator is azodiisobutyronitrile, and the comonomer methacrylic acid, the modifying agent includes plasticizer
And crosslinking agent.
Embodiment 2
The preparation method of the bubble-free lucite tube includes the following steps:
S1: feedstock processing: cleaning methyl methacrylate, obtains clear methyl methacrylate solution, then does
Dry purifying methyl acrylic methylmethacrylate monomer, is cleaned using 10% sodium hydroxide solution and 60% ultrapure water, wash number 5
It is secondary；
S2: step S1 treated methyl methacrylate list prepolymerization: will be added in initiator, comonomer and modifying agent
Body vibrate in heating, and the viscosity no-load voltage ratio of observation liquid, stops when viscosity is close to silicone oil state during oscillation
Heating oscillation, then uses oil bath heated at constant temperature 22 hours, and oil bath heating temperature is 45 degrees Celsius；
S3: rear polymerization: after the completion of oil bath, being put into baking oven, and temperature rises to 100 degrees Celsius, reacts 30 minutes, so that monomer is complete
Full conversion, rear polymerization are completed；
S4: moulding by casting: taking organic glass pipe mold, and the slurry after polymerization is slowly poured in the inner, and casting height control is 8
Centimetre, heating 4 hours in 48-54 degrees Celsius of water-bath are then placed on, organic glass pipe mold is needed before use using baking
Case is preheated, and preheating temperature is 105 degrees Celsius；
S5: heat treatment: after the completion of water-bath, organic glass pipe mold being placed in baking oven and is heat-treated, heat treatment temperature 96
Degree Celsius, heat treatment time is 2 hours；
S6: it demoulding packaging: after the completion of heat treatment, demoulded, polished, polished and is packed.
In the present embodiment, methyl methacrylate: 90 parts；Initiator: 0.15 part；Comonomer: 6 parts and modifying agent:
0.3 part, the initiator be azodiisobutyronitrile, the comonomer methacrylic acid, the modifying agent include plasticizer and
Crosslinking agent.
Embodiment 3
The preparation method of the bubble-free lucite tube includes the following steps:
S1: feedstock processing: cleaning methyl methacrylate, obtains clear methyl methacrylate solution, then does
Dry purifying methyl acrylic methylmethacrylate monomer, is cleaned using 10% sodium hydroxide solution and 60% ultrapure water, wash number 4
It is secondary；
S2: step S1 treated methyl methacrylate list prepolymerization: will be added in initiator, comonomer and modifying agent
Body vibrate in heating, and the viscosity no-load voltage ratio of observation liquid, stops when viscosity is close to silicone oil state during oscillation
Heating oscillation, then uses oil bath heated at constant temperature 20 hours, and oil bath heating temperature is 43 degrees Celsius；
S3: rear polymerization: after the completion of oil bath, being put into baking oven, and temperature rises to 93 degrees Celsius, reacts 25 minutes, so that monomer is complete
Full conversion, rear polymerization are completed；
S4: moulding by casting: taking organic glass pipe mold, and the slurry after polymerization is slowly poured in the inner, and casting height control is 7
Centimetre, heating 3.5 hours in 51 degrees Celsius of water-bath are then placed on, organic glass pipe mold is needed before use using baking oven
It is preheated, preheating temperature is 100 degrees Celsius；
S5: heat treatment: after the completion of water-bath, organic glass pipe mold being placed in baking oven and is heat-treated, heat treatment temperature 90
Degree Celsius, heat treatment time is 1.5 hours；
S6: it demoulding packaging: after the completion of heat treatment, demoulded, polished, polished and is packed.
In the present embodiment, methyl methacrylate: 100 parts；Initiator: 0.137-0.15 parts；Comonomer: 8 parts and
Modifying agent: 0.25 part, the initiator is azodiisobutyronitrile, and the comonomer methacrylic acid, the modifying agent includes
Plasticizer and crosslinking agent.
Lucite tube prepared by above three embodiments is taken to carry out bubble detection, specific testing result please refers to down
Table:
| Number | Number of bubbles (a) | Bubble distribution | Air Bubble Size |
| Embodiment 1 | Few (3) | It is distributed in surface | It is small |
| Embodiment 2 | Less (5) | It is distributed in surface | It is small |
| Embodiment 3 | Nothing | - | - |
In summary, highly preferred embodiment of the present invention be embodiment 3, the bubble-free lucite tube and preparation method thereof,
The vitrifying of lucite tube can be effectively improved by being cross-linked to form space network by introducing polar group by copolymerization
Temperature, and by optimization reaction temperature and initiator amount, it enables to lucite tube to reach hardness and maximizes effect, and energy
It is enough effectively to reduce the bubble generated in decomposable process, and the introducing of bubble can be prevented, improve product light transmittance, the invention
Preparation method is simple, and defect rate is low.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (8)
1. a kind of bubble-free lucite tube, it is characterised in that: the bubble-free lucite tube includes following constituent:
Methyl methacrylate: 90-110 parts；Initiator: 0.125-0.15 parts；Comonomer: 6-10 parts and modifying agent: 0.2-
0.3 part.
2. a kind of bubble-free lucite tube according to claim 1, it is characterised in that: the initiator is that azo two is different
Butyronitrile.
3. a kind of bubble-free lucite tube according to claim 1, it is characterised in that: the comonomer metering system
Acid.
4. a kind of bubble-free lucite tube according to claim 1, it is characterised in that: the modifying agent includes plasticizer
And crosslinking agent.
5. a kind of preparation method of bubble-free lucite tube, it is characterised in that: the preparation method of the bubble-free lucite tube
Include the following steps:
S1: feedstock processing: cleaning methyl methacrylate, obtains clear methyl methacrylate solution, then does
Dry purifying methyl acrylic methylmethacrylate monomer；
S2: step S1 treated methyl methacrylate list prepolymerization: will be added in initiator, comonomer and modifying agent
Body vibrate in heating, and the viscosity no-load voltage ratio of observation liquid, stops when viscosity is close to silicone oil state during oscillation
Heating oscillation, then uses oil bath heated at constant temperature 18-22 hours；
S3: rear polymerization: after the completion of oil bath, being put into baking oven, and temperature rises to 85-100 degrees Celsius, reacts 20-30 minutes, so that
Complete monomer conversion, rear polymerization are completed；
S4: moulding by casting: taking organic glass pipe mold, and the slurry after polymerization is slowly poured in the inner, and casting height control exists
6-8 centimetres, then it is placed on heating 3-4 hours in 48-54 degrees Celsius of water-bath；
S5: heat treatment: after the completion of water-bath, organic glass pipe mold being placed in baking oven and is heat-treated, heat treatment temperature 86-
96 degrees Celsius, heat treatment time is 1-2 hours；
S6: it demoulding packaging: after the completion of heat treatment, demoulded, polished, polished and is packed.
6. a kind of preparation method of bubble-free lucite tube according to claim 5, it is characterised in that: the step S1
In, it is cleaned using 10% sodium hydroxide solution and 60% ultrapure water, wash number is 4-5 times.
7. a kind of preparation method of bubble-free lucite tube according to claim 5, it is characterised in that: the step S2
In oil bath heating temperature be 40-45 degrees Celsius.
8. a kind of preparation method of bubble-free lucite tube according to claim 5, it is characterised in that: the step S4
In, organic glass pipe mold needs to be preheated using baking oven before use, and preheating temperature is 95-105 degrees Celsius.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810928896.8A CN109280122A (en) | 2018-08-15 | 2018-08-15 | A kind of bubble-free lucite tube and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810928896.8A CN109280122A (en) | 2018-08-15 | 2018-08-15 | A kind of bubble-free lucite tube and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN109280122A true CN109280122A (en) | 2019-01-29 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810928896.8A Pending CN109280122A (en) | 2018-08-15 | 2018-08-15 | A kind of bubble-free lucite tube and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110642973A (en) * | 2019-09-27 | 2020-01-03 | 安徽新涛光电科技有限公司 | Method for eliminating shrinkage mark of acrylic casting plate |
| CN111499795A (en) * | 2020-05-07 | 2020-08-07 | 浙江展宇新材料有限公司 | Production process of PMMA monomer copolymerized organic glass |
| CN112142905A (en) * | 2020-10-15 | 2020-12-29 | 天长市蓝天复合材料有限公司 | Method for forming thick-wall organic glass tube |
| CN114854067A (en) * | 2022-05-06 | 2022-08-05 | 董耀武 | Preparation method of glass PMMA micro-nano interface structure laminated material |
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| CN105018007A (en) * | 2015-08-04 | 2015-11-04 | 铱格斯曼航空科技集团有限公司 | Preparation method of aviation organic glass liquid perfusion adhesive |
| 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 |
| CN107099111A (en) * | 2017-04-05 | 2017-08-29 | 浙江龙游展宇有机玻璃有限公司 | A kind of production technology of acryl |
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2018
- 2018-08-15 CN CN201810928896.8A patent/CN109280122A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105018007A (en) * | 2015-08-04 | 2015-11-04 | 铱格斯曼航空科技集团有限公司 | Preparation method of aviation organic glass liquid perfusion adhesive |
| 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 |
| CN107099111A (en) * | 2017-04-05 | 2017-08-29 | 浙江龙游展宇有机玻璃有限公司 | A kind of production technology of acryl |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110642973A (en) * | 2019-09-27 | 2020-01-03 | 安徽新涛光电科技有限公司 | Method for eliminating shrinkage mark of acrylic casting plate |
| CN111499795A (en) * | 2020-05-07 | 2020-08-07 | 浙江展宇新材料有限公司 | Production process of PMMA monomer copolymerized organic glass |
| CN112142905A (en) * | 2020-10-15 | 2020-12-29 | 天长市蓝天复合材料有限公司 | Method for forming thick-wall organic glass tube |
| CN114854067A (en) * | 2022-05-06 | 2022-08-05 | 董耀武 | Preparation method of glass PMMA micro-nano interface structure laminated material |
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Application publication date: 20190129 |