CN112250788A - Method for preparing acrylic thick plate by water bath cooling - Google Patents

Method for preparing acrylic thick plate by water bath cooling Download PDF

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Publication number
CN112250788A
CN112250788A CN202010969974.6A CN202010969974A CN112250788A CN 112250788 A CN112250788 A CN 112250788A CN 202010969974 A CN202010969974 A CN 202010969974A CN 112250788 A CN112250788 A CN 112250788A
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nano
water bath
plate
acrylic
prepolymerization
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朱家兴
朱春燕
陈惠芳
李家许
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Suzhou Xiyake Aquarium Technology Co ltd
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Suzhou Xiyake Aquarium Technology Co ltd
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
    • B29D7/00—Producing flat articles, e.g. films or sheets
    • B29D7/01—Films or sheets
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/04—Ingredients characterised by their shape and organic or inorganic ingredients
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • C08K3/042—Graphene or derivatives, e.g. graphene oxides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/16—Halogen-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/02—Fibres or whiskers
    • C08K7/04—Fibres or whiskers inorganic
    • C08K7/14—Glass
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/16—Halogen-containing compounds
    • C08K2003/162—Calcium, strontium or barium halides, e.g. calcium, strontium or barium chloride
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C08K2003/265—Calcium, strontium or barium carbonate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives

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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)
  • Mechanical Engineering (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Polymerisation Methods In General (AREA)

Abstract

The invention discloses a method for preparing an acrylic thick plate by water bath cooling, which is characterized by comprising the following steps: the method comprises the following steps: 1) prepolymerization pulping, 2) degassing, 3) discharging and injecting, 4) water bath polymerization, 5) demolding, 6) splicing and 7) drying room sizing. The organic glass plate obtained by the formula disclosed by the application has good transparency, the relative density of the organic glass plate is less than half of that of common glass, the crushing resistance of the organic glass plate is several times higher than that of the common glass plate, and the organic glass plate has good electrical insulation and mechanical strength. The acrylic thick plate that this application can obtain, thickness is greater than 100mm, and the luminousness reaches more than 92%.

Description

Method for preparing acrylic thick plate by water bath cooling
Technical Field
The invention belongs to the technical field of organic glass, and particularly relates to a method for preparing an acrylic thick plate by water bath cooling.
Background
Acrylic, also called PMMA or plexiglass, is derived from acrylic (acrylic plastic), commonly known as "specially treated plexiglass," and has the chemical name polymethyl methacrylate. The research and development of acrylic has been over one hundred years.
Acrylic is a polymer thermoplastic material which is developed earlier, the processing and forming are convenient, the forming mode of the acrylic material mainly comprises casting forming and extrusion forming, the acrylic material can be made into various required shapes by reheating and softening the acrylic material after forming, the acrylic material has better transparency and light transmittance, the light transmittance can reach 92 percent, the chemical stability and the weather resistance are better, and the adaptability to the natural environment is strong. But the toughness and the light transmission are slightly insufficient in a high-requirement special use environment, and the use of the acrylic product is directly influenced to a certain extent.
The thickness of the acrylic sheet obtained by one-step molding is generally 30 mm-50 mm, and further processing is needed to obtain the acrylic sheet with the thickness exceeding 50 mm.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: a high-transparency high-strength acrylic sheet is provided.
In order to solve the technical problems, the technical scheme is as follows: a method for preparing an acrylic thick plate by water bath cooling comprises the following steps:
1) prepolymerization pulping: adding methyl cyanoformate, chloromethyl acetate, diethanol dimethacrylate, azodiisobutyronitrile, isooctyl ester and methyl methacrylate monomers into a reaction kettle, heating to keep the temperature at 100-110 ℃, increasing the pressure to 1MPA, and stirring for 1-2 h; adding fluorite powder, nano calcium carbonate, nano graphene, nano silicon carbide, maleic anhydride, trimethoxy silane, stearic acid, nano glass fiber and a flatting agent into a reaction kettle, and continuously stirring for at least 2 hours at the temperature of 150-160 ℃ and the pressure of 3-5 MPa;
2) degassing: after the reaction is finished, the mixture is pumped into a degassing tank for vacuum degassing;
3) discharging and injecting: injecting the cooled liquid polymethyl methacrylate into a mold;
4) water bath polymerization: putting the fixed die into a water pool at 40 +/-5 ℃ for curing, carrying out water bath polymerization for 3-4 days, heating to 100 ℃ through steam after complete polymerization, hardening the surface of the plate, and keeping for at least 12 hours;
5) demolding: after the surface of the plate is hardened, injecting cold water to cool to 30 +/-2 ℃, and demoulding to obtain an acrylic plate with the thickness of 30-50 mm;
6) splicing: cutting and polishing the thin plate, controlling the temperature at 25 +/-2 ℃, bonding the thin plate by using liquid polymethyl methacrylate, and fixing the thin plate by using a clamp;
7) drying room sizing: and controlling the temperature of the bonded plate at 100 +/-5 ℃ for shaping to obtain a thick plate with the thickness of more than 100 mm.
In the step 1), the raw materials for prepolymerization pulping comprise the following components in percentage by mass: 0.5-0.8% of methyl cyanoformate, 0.08-0.15% of azodiisobutyronitrile, 1.5-3% of chloromethyl acetate, 1.5-2% of dimethyl acrylic acid diethanol, 2-3% of fluorite powder, 1-2% of nano calcium carbonate, 2-3% of nano graphene, 10-12% of nano silicon carbide, 0.5-1% of maleic anhydride, 2-5% of isooctyl ester, 0.8-1.5% of trimethoxy silane, 0.6-1.5% of stearic acid, 10-20% of nano glass fiber, 3-5% of flatting agent and 100% of methyl methacrylate monomer.
Further preferably, in the step 1), the raw material for prepolymerization pulping comprises the following components in percentage by mass: 0.5-0.6% of methyl cyanoformate, 0.1-0.12% of azodiisobutyronitrile, 1.5-2% of chloromethyl acetate, 1.8-2% of dimethyl acrylic acid diethanol, 2-2.5% of fluorite powder, 1-1.5% of nano calcium carbonate, 2-2.5% of nano graphene, 11-12% of nano silicon carbide, 0.5-0.8% of maleic anhydride, 2-3% of isooctyl ester, 0.8-1.2% of trimethoxy silane, 0.8-1.2% of stearic acid, 10-15% of nano glass fiber, 3-4% of flatting agent and 100% of methyl methacrylate monomer.
Further preferably, in the step 1), the raw material for prepolymerization pulping comprises the following components in percentage by mass: 0.5% of methyl cyanoformate, 0.12% of azodiisobutyronitrile, 1.5% of chloromethyl acetate, 1.8% of diethyl dimethacrylate, 2.5% of fluorite powder, 1.5% of nano calcium carbonate, 2% of nano graphene, 11% of nano silicon carbide, 0.8% of maleic anhydride, 3% of isooctyl ester, 1.2% of trimethoxy silane, 0.8% of stearic acid, 12% of nano glass fiber, 3% of flatting agent and 100% of methyl methacrylate monomer.
Further preferably, in the step 1), the raw material for prepolymerization pulping comprises the following components in percentage by mass: 0.6% of methyl cyanoformate, 0.1% of azodiisobutyronitrile, 2% of chloromethyl acetate, 2% of dimethyl acrylic acid diethanol, 2% of fluorite powder, 1% of nano calcium carbonate, 2.5% of nano graphene, 12% of nano silicon carbide, 0.5% of maleic anhydride, 2% of isooctyl ester, 1% of trimethoxy silane, 1.2% of stearic acid, 15% of nano glass fiber, 4% of flatting agent and 100% of methyl methacrylate monomer.
Has the advantages that: the organic glass plate obtained by the formula disclosed by the application has good transparency, the relative density of the organic glass plate is less than half of that of common glass, the crushing resistance of the organic glass plate is several times higher than that of the common glass plate, and the organic glass plate has good electrical insulation and mechanical strength. The acrylic thick plate that this application can obtain, thickness is greater than 100mm, and the luminousness reaches more than 92%.
Detailed Description
The process of the present invention is further illustrated below with reference to examples, but the invention is not limited thereto.
A method for preparing an acrylic thick plate by water bath cooling is characterized by comprising the following steps: the method comprises the following steps:
1) prepolymerization pulping: adding methyl cyanoformate, chloromethyl acetate, diethanol dimethacrylate, azodiisobutyronitrile, isooctyl ester and methyl methacrylate monomers into a reaction kettle, heating to keep the temperature at 100-110 ℃, increasing the pressure to 1MPA, and stirring for 1-2 h; adding fluorite powder, nano calcium carbonate, nano graphene, nano silicon carbide, maleic anhydride, trimethoxy silane, stearic acid, nano glass fiber and a flatting agent into a reaction kettle, and continuously stirring for at least 2 hours at the temperature of 150-160 ℃ and the pressure of 3-5 MPa;
2) degassing: after the reaction is finished, the mixture is pumped into a degassing tank for vacuum degassing;
3) discharging and injecting: injecting the cooled liquid polymethyl methacrylate into a mold;
4) water bath polymerization: putting the fixed die into a water pool at 40 +/-5 ℃ for curing, carrying out water bath polymerization for 3-4 days, heating to 100 ℃ through steam after complete polymerization, hardening the surface of the plate, and keeping for at least 12 hours;
5) demolding: after the surface of the plate is hardened, injecting cold water to cool to 30 +/-2 ℃, and demoulding to obtain an acrylic plate with the thickness of 30-50 mm;
6) splicing: cutting and polishing the thin plate, controlling the temperature at 25 +/-2 ℃, bonding the thin plate by using liquid polymethyl methacrylate, and fixing the thin plate by using a clamp;
7) drying room sizing: and controlling the temperature of the bonded plate at 100 +/-5 ℃ for shaping to obtain a thick plate with the thickness of more than 100 mm.
The raw materials for prepolymerization pulping have the compounding proportion of unit kg.
Figure RE-GDA0002805861180000041
Figure RE-GDA0002805861180000051
Light transmittance: the light transmittance reaches more than 92 percent;
acrylic density: 1.19kg/dm3Impact strength: 16kg/cm3(approximately 16 times stronger than glass), tensile strength: not less than 61kg/cm3The hot bending temperature: not less than 78 ℃; acrylic thickness: is greater than 100 mm.

Claims (5)

1. A method for preparing an acrylic thick plate by water bath cooling is characterized by comprising the following steps: the method comprises the following steps:
1) prepolymerization pulping: adding methyl cyanoformate, chloromethyl acetate, diethanol dimethacrylate, azodiisobutyronitrile, isooctyl ester and methyl methacrylate monomers into a reaction kettle, heating to keep the temperature at 100-110 ℃, increasing the pressure to 1MPA, and stirring for 1-2 h; adding fluorite powder, nano calcium carbonate, nano graphene, nano silicon carbide, maleic anhydride, trimethoxy silane, stearic acid, nano glass fiber and a flatting agent into a reaction kettle, and continuously stirring for at least 2 hours at the temperature of 150-160 ℃ and the pressure of 3-5 MPa;
2) degassing: after the reaction is finished, the mixture is pumped into a degassing tank for vacuum degassing;
3) discharging and injecting: injecting the cooled liquid polymethyl methacrylate into a mold;
4) water bath polymerization: putting the fixed die into a water pool at 40 +/-5 ℃ for curing, carrying out water bath polymerization for 3-4 days, heating to 100 ℃ through steam after complete polymerization, hardening the surface of the plate, and keeping for at least 12 hours;
5) demolding: after the surface of the plate is hardened, injecting cold water to cool to 30 +/-2 ℃, and demoulding to obtain an acrylic plate with the thickness of 30-50 mm;
6) splicing: cutting and polishing the thin plate, controlling the temperature at 25 +/-2 ℃, bonding the thin plate by using liquid polymethyl methacrylate, and fixing the thin plate by using a clamp;
7) drying room sizing: and controlling the temperature of the bonded plate at 100 +/-5 ℃ for shaping to obtain a thick plate with the thickness of more than 100 mm.
2. The method for preparing acrylic thick plates by water bath cooling as claimed in claim 1, wherein the method comprises the following steps: in the step 1), the raw materials for prepolymerization pulping comprise the following components in percentage by mass: 0.5-0.8% of methyl cyanoformate, 0.08-0.15% of azodiisobutyronitrile, 1.5-3% of chloromethyl acetate, 1.5-2% of dimethyl acrylic acid diethanol, 2-3% of fluorite powder, 1-2% of nano calcium carbonate, 2-3% of nano graphene, 10-12% of nano silicon carbide, 0.5-1% of maleic anhydride, 2-5% of isooctyl ester, 0.8-1.5% of trimethoxy silane, 0.6-1.5% of stearic acid, 10-20% of nano glass fiber, 3-5% of flatting agent and 100% of methyl methacrylate monomer.
3. The method for preparing acrylic thick plates by water bath cooling as claimed in claim 2, wherein the method comprises the following steps: in the step 1), the raw materials for prepolymerization pulping comprise the following components in percentage by mass: 0.5-0.6% of methyl cyanoformate, 0.1-0.12% of azodiisobutyronitrile, 1.5-2% of chloromethyl acetate, 1.8-2% of dimethyl acrylic acid diethanol, 2-2.5% of fluorite powder, 1-1.5% of nano calcium carbonate, 2-2.5% of nano graphene, 11-12% of nano silicon carbide, 0.5-0.8% of maleic anhydride, 2-3% of isooctyl ester, 0.8-1.2% of trimethoxy silane, 0.8-1.2% of stearic acid, 10-15% of nano glass fiber, 3-4% of flatting agent and 100% of methyl methacrylate monomer.
4. The method for preparing acrylic slabs by water bath cooling as claimed in claim 3, wherein: in the step 1), the raw materials for prepolymerization pulping comprise the following components in percentage by mass: 0.5% of methyl cyanoformate, 0.12% of azodiisobutyronitrile, 1.5% of chloromethyl acetate, 1.8% of diethyl dimethacrylate, 2.5% of fluorite powder, 1.5% of nano calcium carbonate, 2% of nano graphene, 11% of nano silicon carbide, 0.8% of maleic anhydride, 3% of isooctyl ester, 1.2% of trimethoxy silane, 0.8% of stearic acid, 12% of nano glass fiber, 3% of flatting agent and 100% of methyl methacrylate monomer.
5. The method for preparing acrylic slabs by water bath cooling as claimed in claim 3, wherein: in the step 1), the raw materials for prepolymerization pulping comprise the following components in percentage by mass: 0.6% of methyl cyanoformate, 0.1% of azodiisobutyronitrile, 2% of chloromethyl acetate, 2% of dimethyl acrylic acid diethanol, 2% of fluorite powder, 1% of nano calcium carbonate, 2.5% of nano graphene, 12% of nano silicon carbide, 0.5% of maleic anhydride, 2% of isooctyl ester, 1% of trimethoxy silane, 1.2% of stearic acid, 15% of nano glass fiber, 4% of flatting agent and 100% of methyl methacrylate monomer.
CN202010969974.6A 2020-09-16 2020-09-16 Method for preparing acrylic thick plate by water bath cooling Pending CN112250788A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108003536A (en) * 2017-12-25 2018-05-08 温州中祥光电科技发展有限公司 A kind of high printing opacity acryl plates and preparation method thereof
CN109438615A (en) * 2018-11-15 2019-03-08 张金娥 High-intensitive acryl plates and its preparation process
CN110181838A (en) * 2019-07-05 2019-08-30 浙江横海科技有限公司 Underwater uniform thickness acrylic hemisphere production method
CN112223794A (en) * 2020-09-10 2021-01-15 苏州西雅克水族科技有限公司 Bending and shaping method for acrylic thick plate

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108003536A (en) * 2017-12-25 2018-05-08 温州中祥光电科技发展有限公司 A kind of high printing opacity acryl plates and preparation method thereof
CN109438615A (en) * 2018-11-15 2019-03-08 张金娥 High-intensitive acryl plates and its preparation process
CN110181838A (en) * 2019-07-05 2019-08-30 浙江横海科技有限公司 Underwater uniform thickness acrylic hemisphere production method
CN112223794A (en) * 2020-09-10 2021-01-15 苏州西雅克水族科技有限公司 Bending and shaping method for acrylic thick plate

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Application publication date: 20210122