CN105647141A - Preparation method of flame-retardant resin - Google Patents
Preparation method of flame-retardant resin Download PDFInfo
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- CN105647141A CN105647141A CN201610221306.9A CN201610221306A CN105647141A CN 105647141 A CN105647141 A CN 105647141A CN 201610221306 A CN201610221306 A CN 201610221306A CN 105647141 A CN105647141 A CN 105647141A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/06—Unsaturated polyesters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/52—Polycarboxylic acids or polyhydroxy compounds in which at least one of the two components contains aliphatic unsaturation
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- 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
- C08K3/36—Silica
-
- 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
- C08K5/098—Metal salts of carboxylic acids
-
- 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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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)
- Macromonomer-Based Addition Polymer (AREA)
Abstract
The invention relates to a preparation method a flame-retardant resin. The preparation method adopts crosslinking chemical reaction, and comprises the following steps: (1) at normal temperature, weighing all the raw materials according to parts by weight for later use; (2) at normal temperature, dissolving maleic anhydride, tetrachloro phthalic anhydride, neopentyl glycol, a curing agent chlorinated styrene and methyl methacrylate, and uniformly mixing by sufficient stirring; (3) curing: curing the uniformly mixed solution obtained in the step (2) to obtain an unsaturated polyester resin, wherein the initial curing temperature is 20-30 DEG C, the initial curing time is 10-30 hours, the postcuring temperature is 25-35 DEG C, and the postcuring time is 4-6 hours; and (4) at normal temperature, mixing and dissolving fibers, copper naphthenate, cobalt isooctoate, calcium carbonate and silicon dioxide in the unsaturated polyester resin prepared in the step (3), uniformly mixing by sufficient stirring, and aging at 25 DEG C for at least 36 hours to obtain the flame-retardant resin.
Description
Technical field
The present invention relates to technical field of polymer composite materials, particularly to a kind of flame-retarded resin field.
Background technology
Along with the raising of the development of corrosion and protection and industrialization degree, the application of composite is also increasingly wider, applying working condition, and medium becomes increasingly complex, and uses temperature also more and more higher, and market is also more and more higher to the requirement of its performance. But, owing to phosphorus system (phosphate ester etc.) anti-flammability PC resin and anti-flammability PC/ABS alloy have in a large number the phosphorus flame retardant being added into of (several weight %��more than 10 weight %), therefore there are some problems: when mould injection moulding it may happen that the generation of gas, and when recirculation or placement (for high temperature and high humidity) when accelerated deterioration, the physical property of resin is remarkably decreased; These problems can be attributed to phosphorus flame retardant makes PC composition be hydrolyzed, particularly under high temperature and super-humid conditions.
At present, domestic and international field adopts high-property resin composite material material more single, mainly based on unsaturated polyester (UP), vinyl ester resin, tough epoxy resin material, but these materials Shortcomings part all in various degree; Such as unsaturated polyester (UP), fragility is big, uses temperature low, and adhesive strength is low; Although it is good that vinyl ester resin has good toughness, adhesive strength, the advantages such as after solidification toxicity is little, but exist and use the shortcomings such as temperature is low; Epoxy resin, although having good toughness, adhesive strength advantages of higher, but there is weatherability difference, easy efflorescence, viscosity is big, wettability is poor, at relatively high temperatures, bearing poor compared with the ability of strong corrosive medium such as stronger acids, alkali and solvent etc., curing system toxicity is big, the shortcomings such as cure cycle is long, and post-treatment expense is high. Therefore, the requirement that traditional composite is increasingly higher to its performance far from meeting market.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of normal temperature solidified and solidifies avirulence, product long service life, the flame-retarded resin that heat-resistant fireproof excellent performance, adhesive strength are high.
In order to solve above-mentioned technical problem, the technical solution used in the present invention is, this flame-retarded resin, including the component of following mass fraction: chloro styrene 10 ~ 20 parts, maleic anhydride 10 ~ 15 parts, tetrachlorophthalic anhydride 20 ~ 30 parts, neopentyl glycol 40 ~ 55 parts, methyl methacrylate 2 ~ 7 parts, fiber 8 ~ 15 parts, copper naphthenate 6 ~ 10 parts, cobalt iso-octoate 1 ~ 3 part, calcium carbonate 20 ~ 30 parts, silicon dioxide 8 ~ 12 parts.
Preferred version as the present invention, component including following mass fraction: chloro styrene 16 parts, maleic anhydride 10 parts, tetrachlorophthalic anhydride 30 parts, neopentyl glycol 48 parts, methyl methacrylate 4 parts, fiber 10 parts, copper naphthenate 8 parts, cobalt iso-octoate 2 parts, calcium carbonate 23 parts, silica 10 part.
By technique scheme, employing tetrachlorophthalic anhydride is raw material, it is possible to strengthen the anti-flammability of resin, simultaneously with chloro styrene for firming agent, further enhances the anti-flammability of resin; In addition obtained flame retardant resin has high temperature resistant, corrosion-resistant, high intensity, product long service life, processing technique is simple and normal temperature solidified, solidify avirulence, adhesive strength high, not only technological process is simply controlled, with short production cycle, and in resin synthesis process, make full use of chemical reaction produce heat, the energy-conservation energy and without the three wastes produce.
The present invention also to solve the technical problem that and is to provide a kind of normal temperature solidified and solidifies avirulence, product long service life, the preparation method of the flame-retarded resin that heat-resistant fireproof excellent performance, adhesive strength are high.
In order to solve above-mentioned technical problem, the technical solution used in the present invention is, the preparation method of flame-retarded resin specifically comprises the following steps that
(1) at normal temperatures, all raw material is weighed by weight ratio, stand-by;
(2) after at normal temperatures, maleic anhydride, tetrachlorophthalic anhydride, neopentyl glycol and firming agent chloro styrene and methyl methacrylate being dissolved and mixing be sufficiently stirred for again and make its mix homogeneously;
(3) solidify: being solidified by the solution of the mix homogeneously of step (2) gained, initial curing temperature is 20 ~ 30 DEG C, and initial setting time is 10 ~ 30 hours; Rear solidification temperature is 25 ~ 35 DEG C, and rear curing time is 4 ~ 6 hours, prepares unsaturated polyyester;
(4) at normal temperatures, after the unsaturated polyyester mixed dissolution obtained with step (3) by fiber, copper naphthenate, cobalt iso-octoate, calcium carbonate and silicon dioxide and be sufficiently stirred for and make it mix homogeneously, then at 25 DEG C, namely maintenance obtained flame-retarded resin after at least 36 hours.
This resin viscosity is moderate, and adhesive strength is high; After post curing treatment, it is possible to effectively eliminate internal stress.
Detailed description of the invention
Embodiment 1: proportioning raw materials is: chloro styrene 16 parts, maleic anhydride 10 parts, tetrachlorophthalic anhydride 30 parts, neopentyl glycol 48 parts, methyl methacrylate 4 parts, fiber 10 parts, copper naphthenate 8 parts, cobalt iso-octoate 2 parts, calcium carbonate 23 parts, silica 10 part;
Concrete preparation process is as follows:
(1) at normal temperatures, all raw material is weighed by weight ratio, stand-by;
(2) after at normal temperatures, maleic anhydride, tetrachlorophthalic anhydride, neopentyl glycol and firming agent chloro styrene and methyl methacrylate being dissolved and mixing be sufficiently stirred for again and make its mix homogeneously;
(3) solidify: being solidified by the solution of the mix homogeneously of step (2) gained, initial curing temperature is 25 DEG C, and initial setting time is 20 hours; Rear solidification temperature is 30 DEG C, and rear curing time is 5 hours, prepares unsaturated polyyester;
(4) at normal temperatures, after the unsaturated polyyester mixed dissolution obtained with step (3) by fiber, copper naphthenate, cobalt iso-octoate, calcium carbonate and silicon dioxide and be sufficiently stirred for and make it mix homogeneously, then at 25 DEG C, namely maintenance obtained flame-retarded resin after 40 hours.
Embodiment 2:
Proportioning raw materials is: chloro styrene 10 parts, maleic anhydride 10 parts, tetrachlorophthalic anhydride 30 parts, neopentyl glycol 40 parts, methyl methacrylate 7 parts, fiber 8 parts, copper naphthenate 10 parts, cobalt iso-octoate 3 parts, calcium carbonate 20 parts, silica 12 parts;
Concrete preparation process is as follows:
(1) at normal temperatures, all raw material is weighed by weight ratio, stand-by;
(2) after at normal temperatures, maleic anhydride, tetrachlorophthalic anhydride, neopentyl glycol and firming agent chloro styrene and methyl methacrylate being dissolved and mixing be sufficiently stirred for again and make its mix homogeneously;
(3) solidify: being solidified by the solution of the mix homogeneously of step (2) gained, initial curing temperature is 20 DEG C, and initial setting time is 30 hours; Rear solidification temperature is 25 DEG C, and rear curing time is 6 hours, prepares unsaturated polyyester;
(4) at normal temperatures, after the unsaturated polyyester mixed dissolution obtained with step (3) by fiber, copper naphthenate, cobalt iso-octoate, calcium carbonate and silicon dioxide and be sufficiently stirred for and make it mix homogeneously, then at 25 DEG C, namely maintenance obtained flame-retarded resin after 48 hours.
Embodiment 3: proportioning raw materials is: chloro styrene 20 parts, maleic anhydride 15 parts, tetrachlorophthalic anhydride 20 parts, neopentyl glycol 55 parts, methyl methacrylate 2 parts, fiber 15 parts, copper naphthenate 6 parts, cobalt iso-octoate 1 part, calcium carbonate 30 parts, silicon dioxide 8 parts;
Concrete preparation process is as follows:
(1) at normal temperatures, all raw material is weighed by weight ratio, stand-by;
(2) after at normal temperatures, maleic anhydride, tetrachlorophthalic anhydride, neopentyl glycol and firming agent chloro styrene and methyl methacrylate being dissolved and mixing be sufficiently stirred for again and make its mix homogeneously;
(3) solidify: being solidified by the solution of the mix homogeneously of step (2) gained, initial curing temperature is 30 DEG C, and initial setting time is 10 hours; Rear solidification temperature is 35 DEG C, and rear curing time is 4 hours, prepares unsaturated polyyester;
(4) at normal temperatures, after the unsaturated polyyester mixed dissolution obtained with step (3) by fiber, copper naphthenate, cobalt iso-octoate, calcium carbonate and silicon dioxide and be sufficiently stirred for and make it mix homogeneously, then at 25 DEG C, namely maintenance obtained flame-retarded resin after 40 hours.
Finally, in addition it is also necessary to be only several specific embodiments of the present invention it is noted that listed above. It is clear that the invention is not restricted to above example, it is also possible to there are many deformation. All deformation that those of ordinary skill in the art can directly derive from present disclosure or associate, are all considered as protection scope of the present invention.
Claims (1)
1. a preparation method for flame-retarded resin, adopts cross-linking chemistry reaction, specifically comprises the following steps that
(1) at normal temperatures, all raw material is weighed by weight ratio, stand-by;
(2) after at normal temperatures, maleic anhydride, tetrachlorophthalic anhydride, neopentyl glycol and firming agent chloro styrene and methyl methacrylate being dissolved and mixing be sufficiently stirred for again and make its mix homogeneously;
(3) solidify: being solidified by the solution of the mix homogeneously of step (2) gained, initial curing temperature is 20 ~ 30 DEG C, and initial setting time is 10 ~ 30 hours; Rear solidification temperature is 25 ~ 35 DEG C, and rear curing time is 4 ~ 6 hours, prepares unsaturated polyyester;
(4) at normal temperatures, after the unsaturated polyyester mixed dissolution obtained with step (3) by fiber, copper naphthenate, cobalt iso-octoate, calcium carbonate and silicon dioxide and be sufficiently stirred for and make it mix homogeneously, then at 25 DEG C, namely maintenance obtained flame-retarded resin after at least 36 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610221306.9A CN105647141A (en) | 2016-04-12 | 2016-04-12 | Preparation method of flame-retardant resin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610221306.9A CN105647141A (en) | 2016-04-12 | 2016-04-12 | Preparation method of flame-retardant resin |
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| CN105647141A true CN105647141A (en) | 2016-06-08 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109233544A (en) * | 2017-05-17 | 2019-01-18 | 无锡市银杏塑业科技有限公司 | A kind of resistance to jelly resin |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102219882A (en) * | 2011-05-04 | 2011-10-19 | 肇庆福田化学工业有限公司 | Method for synthesizing unsaturated polyester resin by utilizing glycerol |
| CN102558800A (en) * | 2010-12-25 | 2012-07-11 | 李霞 | Flame-retarded resin |
| CN105085885A (en) * | 2015-09-21 | 2015-11-25 | 永悦科技股份有限公司 | Colorant matrix resin for unsaturated polyester resin and preparation method thereof |
-
2016
- 2016-04-12 CN CN201610221306.9A patent/CN105647141A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102558800A (en) * | 2010-12-25 | 2012-07-11 | 李霞 | Flame-retarded resin |
| CN102219882A (en) * | 2011-05-04 | 2011-10-19 | 肇庆福田化学工业有限公司 | Method for synthesizing unsaturated polyester resin by utilizing glycerol |
| CN105085885A (en) * | 2015-09-21 | 2015-11-25 | 永悦科技股份有限公司 | Colorant matrix resin for unsaturated polyester resin and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109233544A (en) * | 2017-05-17 | 2019-01-18 | 无锡市银杏塑业科技有限公司 | A kind of resistance to jelly resin |
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Application publication date: 20160608 |