CN105647097A - Flame-retardant resin - Google Patents
Flame-retardant resin Download PDFInfo
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- CN105647097A CN105647097A CN201610221250.7A CN201610221250A CN105647097A CN 105647097 A CN105647097 A CN 105647097A CN 201610221250 A CN201610221250 A CN 201610221250A CN 105647097 A CN105647097 A CN 105647097A
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- resin
- flame
- calcium carbonate
- methyl methacrylate
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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
- 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
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/01—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to unsaturated polyesters
-
- 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
- C08G63/68—Polyesters containing atoms other than carbon, hydrogen and oxygen
- C08G63/682—Polyesters containing atoms other than carbon, hydrogen and oxygen containing halogens
- C08G63/6824—Polyesters containing atoms other than carbon, hydrogen and oxygen containing halogens derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/6828—Polycarboxylic acids and polyhydroxy compounds in which at least one of the two components contains aliphatic unsaturation
-
- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
-
- 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
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
-
- 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)
- Adhesives Or Adhesive Processes (AREA)
- Macromonomer-Based Addition Polymer (AREA)
Abstract
The invention relates to a flame-retardant resin which comprises the following components in parts by mass: 10-20 parts of chlorinated styrene, 10-15 parts of maleic anhydride, 20-30 parts of tetrachloro phthalic anhydride, 40-55 parts of neopentyl glycol, 2-7 parts of methyl methacrylate, 8-15 parts of fiber, 6-10 parts of copper naphthenate, 1-3 parts of cobalt isooctoate, 20-30 parts of calcium carbonate and 8-12 parts of silicon dioxide. The tetrachloro phthalic anhydride used as the raw material can enhance the flame retardancy of the resin, and the chlorinated styrene used as the curing agent further enhances the flame retardancy of the resin. The flame-retardant resin has the characteristics of high temperature resistance, corrosion resistance, high strength, long service life of the prepared part, simple processing technique, no toxicity after curing, high bonding strength, simple and controllable technical process, short production cycle and the like, and can be cured at normal temperature. In the resin synthesis process, the heat generated by chemical reaction is fully utilized, thereby saving the energy and avoiding generating three wastes.
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 (2)
1. a flame-retarded resin, it is characterized in that, component including 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.
2. flame-retarded resin according to claim 1, it is characterized in that, 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610221250.7A CN105647097A (en) | 2016-04-12 | 2016-04-12 | Flame-retardant resin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610221250.7A CN105647097A (en) | 2016-04-12 | 2016-04-12 | Flame-retardant resin |
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| Publication Number | Publication Date |
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| CN105647097A true CN105647097A (en) | 2016-06-08 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610221250.7A Pending CN105647097A (en) | 2016-04-12 | 2016-04-12 | Flame-retardant resin |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106751796A (en) * | 2016-11-28 | 2017-05-31 | 天津映之科技有限公司 | A kind of composite material and preparation method thereof |
| CN108559231A (en) * | 2018-03-27 | 2018-09-21 | 湖州五石科技有限公司 | A kind of flame-retarded resin |
| CN108789758A (en) * | 2018-06-29 | 2018-11-13 | 怀宁县科林木业有限公司 | The particieboard processing method of highly effective flame-retardant |
| CN110128600A (en) * | 2019-05-21 | 2019-08-16 | 河南省华昌高新技术有限公司 | A kind of flame-retarded resin and preparation method thereof |
Citations (5)
| 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 |
| CN103540112A (en) * | 2013-10-19 | 2014-01-29 | 山东吉青化工有限公司 | High-temperature-resistant flame-retardant resin |
| CN103602049A (en) * | 2013-10-30 | 2014-02-26 | 山东吉青化工有限公司 | Flame-retardant 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 CN201610221250.7A patent/CN105647097A/en active Pending
Patent Citations (5)
| 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 |
| CN103540112A (en) * | 2013-10-19 | 2014-01-29 | 山东吉青化工有限公司 | High-temperature-resistant flame-retardant resin |
| CN103602049A (en) * | 2013-10-30 | 2014-02-26 | 山东吉青化工有限公司 | Flame-retardant 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 |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106751796A (en) * | 2016-11-28 | 2017-05-31 | 天津映之科技有限公司 | A kind of composite material and preparation method thereof |
| CN108559231A (en) * | 2018-03-27 | 2018-09-21 | 湖州五石科技有限公司 | A kind of flame-retarded resin |
| CN108789758A (en) * | 2018-06-29 | 2018-11-13 | 怀宁县科林木业有限公司 | The particieboard processing method of highly effective flame-retardant |
| CN110128600A (en) * | 2019-05-21 | 2019-08-16 | 河南省华昌高新技术有限公司 | A kind of flame-retarded resin and preparation method thereof |
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Application publication date: 20160608 |
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