CN107603116A - Mold pressing resin and preparation method thereof - Google Patents
Mold pressing resin and preparation method thereof Download PDFInfo
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- CN107603116A CN107603116A CN201610548076.7A CN201610548076A CN107603116A CN 107603116 A CN107603116 A CN 107603116A CN 201610548076 A CN201610548076 A CN 201610548076A CN 107603116 A CN107603116 A CN 107603116A
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Abstract
The invention discloses a kind of mold pressing resin to also disclose a kind of preparation method of mold pressing resin, and its drip irrigation device is made of mainly by the raw material of following percentage：Diethylene glycol (DEG) 19.4 20, phthalic anhydride 7 7.6, cis-butenedioic anhydride 27.5 28.5, neopentyl glycol 13.8 14.5, styrene 25 30, polymerization inhibitor 0.009, antioxidant 0.01 0.015, retarder 0.003 0.031, plasticizer 0.025 0.028, chelating agent 25.The mold pressing resin of the present invention has the advantages of combination property is stronger.
Description
Technical field
The present invention relates to chemical field, more particularly to a kind of mold pressing resin and preparation method thereof.
Background technology
Unsaturated polyester resin (UnsaturatedPolyesterResins, abbreviation UPR) is the line for having function groups
Type high-molecular compound, there is polyester chain link and unsaturated double-bond on its skeleton main chain, and respectively carried at macromolecular chain both ends
Carboxyl and hydroxyl.The use of the maximum benefit of unsaturated polyester resin is that its diluent (styrene) will and be led in last use
Double bond on chain is copolymerized cross-linking reaction, so the volatile quantity of solvent is less during use, thus belongs to environmental protection one
The product of class, often it is that matrix is used for SMC/BMC arts by the product.
BMC, also referred to as glass fiber reinforced unsaturated polyester plastic.Its main raw material(s) is by staple glass
The bulk prepreg that fiber, unsaturated polyester resin, filler and various additives are adequately mixed.Belong to thermosetting mould
One kind in plastic shaping material, mainly using fields such as electrical engineering and electric apparatus, motor, automobile, building, daily necessities.
Sheet molding compound is to impregnate fiber or chopped mat by resin paste, both sides covering polyethylene film and manufactured one
Class sheet molding compound, belong to prepreg mat material scope, be one of current moulding material most widely used in the world.
Although sheet molding compound and block molding compound are by the continuous development and improvement of decades, the batch matter of product
Amount it is still unstable, fill its reason mainly due to matrix resin later stage thicken slowly and thicken it is unstable caused by.
Existing mold pressing resin, a kind of unsaturated polyester resin for mould pressing as disclosed in Application No. 201110061600.5
And preparation method thereof, the invention discloses a kind of unsaturated polyester resin for mould pressing and preparation method thereof, the resin mainly by with
The raw material composition of lower parts by weight：The parts by weight of phthalic anhydride 120~150, the parts by weight of propane diols 290~350, the weight of cis-butenedioic anhydride 440~470
Part, the parts by weight of DPG 70~100, the parts by weight of methyl propanediol 40~50, the parts by weight of neopentyl glycol 70~85, styrene
420~470 parts by weight.The mold pressing resin improves thickening stabilities and later stage thickening speed, but tensile strength, bending are by force
Degree and bus hardness is not high.
The content of the invention
The purpose of the present invention one is to provide a kind of mold pressing resin, and it has the advantages of combination property is more preferable.
The present invention above-mentioned technical purpose one technical scheme is that：A kind of mold pressing resin, mainly
It is made up of the raw material of following mass percent：Diethylene glycol (DEG) 19.4-20, phthalic anhydride 7-7.6, cis-butenedioic anhydride 27.5-28.5, neopentyl glycol
13.8-14.5, styrene 25-30, polymerization inhibitor 0.009, antioxidant 0.01-0.015, retarder 0.003-0.031, plasticizer
0.025-0.028, chelating agent 2-5.
By using above-mentioned technical proposal, chelating agent can improve dispersibility so that each component mixes more equal
Even, invention changes the ratio of macromolecular chain end carboxyl and hydroxyl in resin, improves the content of macromolecular chain end carboxyl, is solved with this
The defects of thickening of globs of material later stage is slow, the free acid content reduced in resin bring instable influence to globs of material thickening,
The thickening characteristic of batch dough is promoted to tend towards stability.In addition, the present invention abandons traditional methyl propanediol and 1,2-PD, adopt
With substantial amounts of diethylene glycol (DEG), toughness is not only increased, cost is also significantly reduced and also improves tensile strength height, bending by force
Degree, bus hardness, improve the combination property of the mold pressing resin.
As preferable, the resin is mainly made up of the raw material of following mass percent：Diethylene glycol (DEG) 19.7, phthalic anhydride 7.5 are suitable
Acid anhydride 27, neopentyl glycol 14, styrene 31.5, polymerization inhibitor 0.009, antioxidant 0.01, retarder 0.003, plasticizer 0.025, chela
Mixture 2.
Mainly it is made up of as preferable, described antioxidant the raw material of following mass percent：Dibutyl dithio ammonia
Base zinc formate 0.1-0.3；Amino-pyrazol 0.01-0.06；Acetyl acetone 0.01-0.02；Dihydroxy benaophenonel 0.01-0.02；
Loop coil ethylene glycol 0.01-0.02；Polyolefine powder 98-99.6.
By using above-mentioned technical proposal, the antioxidant has the feature of environmental protection, hydrolytic resistance, and resistance to elevated temperatures alleviates the resin
Reaction speed and alleviate the resin degradation with aging, the tensile strength for also improving the mold pressing resin is high, bending strength is good, bar
Scholar's hardness is strong.
It is made up of as preferable, described plasticizer the composition of following mass percent：Fatty acid methyl ester 10-20；Ring
Oxygen fatty acid methyl ester 20-30；Benzoic acid 5-8；Activated carbon 1.4-1.6；The 4-5 of phosphinylidyne two；Soluble polyvinyl alcohol 5-8；Epoxy soybean
Oily 10-15；Ethylene glycol 5-10；Isononyl alcohol 5-10；Magnesia 0.4-0.6；Epoxy palm oil 9-12, roseolic acid 3-6.
By using above-mentioned technical proposal, epoxidized soybean oil and epoxy palm oil are regarded as nontoxic plasticiser, medium
Viscosity, high stability, therefore the increase activated carbon composition that can improve the mold pressing resin can be adsorbed because of murder by poisoning caused by reaction
Gas.
It is arene nitro compound polymerization inhibitor as preferable, described polymerization inhibitor.
It is copper naphthenate as preferable, described retarder.
As one kind that preferable, described chelating agent is amino carboxylic acid or 1,3- diketone.
The purpose of the present invention two is to provide a kind of preparation method of mold pressing resin, and the mold pressing resin that this method is prepared has
The advantages of combination property is stronger.
The present invention above-mentioned technical purpose two technical scheme is that：A kind of preparation of mold pressing resin
Method, comprise the following steps：
A) diethylene glycol (DEG), phthalic anhydride, cis-butenedioic anhydride, diethylene glycol, neopentyl glycol, antioxidant and 2/3 chelating agent are put into reaction successively
In kettle, reaction is started to warm up, when kettle temperature reaches 120-140 DEG C, starts to stir；
B) under conditions of nitrogen flow is 6~10m3/h, control and evaporate 100-105 DEG C of a temperature, after 1~1.5h of insulation reaction,
Voluntarily heat release to 140 DEG C, is warming up to 180 DEG C, then be warming up to 190 with 4~5 DEG C/h speed with 18~20 DEG C/h speed for reaction
DEG C, finally it is warming up to 200 DEG C with 9~10 DEG C/h speed；
C) adjust to void tower, nitrogen flow and increase to 85-90m/h, react to acid number 28-37mKOH/g, nitrogen flow is adjusted
To 10~15m3/h, cooling, when temperature of charge is down to 180 DEG C, polymerization inhibitor is added, be down to 170~175 DEG C and obtain molding tree
Fat；
D) add remaining chelating agent and carry out cooling dilution, carry out being cooled to 80 DEG C；
E) under conditions of temperature is less than 80 DEG C, dilution kettle squeezes into plasticizer, retarder and styrene in advance, stirs 30min
More than.
As preferential, insulation reaction 3~5.5 hours under the conditions of step b) is additionally included in 200 DEG C, react to acid number up to 60
~70mgKOH/g, nitrogen flow is adjusted to 60~80m3/h, reacted to acid number up to 40~45mgKOH/g.
As preferential, in step d), after material cooling first is diluted into 175 DEG C, with 5-10 DEG C per hour of speed
Carry out being cooled to 80 DEG C.
By using above-mentioned technical proposal, the present invention is prevented incorrect using appropriate polymerization inhibitor and specific feed postition
Polymerization and influence reaction speed.Moreover, in preparation process, acid number is first controlled preferably between 60~70mgKOH/g, if acid number
Too high, free acid or acid are more, are easily lost in；If acid number is too low, can lose time significantly, then the nitrogen using appropriate flow velocity
Gas re-adjustments acid number is in 40-45mgKOH/g.Using the nitrogen of appropriate flow velocity, beneficial to moisture content is carried, contribute to entering for reaction
OK.Heating when use gradient increased temperature, be when being rapidly heated from 140 DEG C to 180 DEG C guarantee be rapidly achieved the boiling point of alcohol before,
180 DEG C slow down when being warming up to 190 DEG C to ensure that alcohol reaction is complete, avoid losing, and are warming up to 200 at a given speed again
DEG C it is to ensure to be converted to sour regurgitation along acid, adjusts to void tower and then adjust again the flow velocity of nitrogen, will to realize regulation acid number
It is controlled in 28-37mKOH/g, is then adjusted the flow velocity of nitrogen again and is down to proper temperature addition polymerization inhibitor and continues to react,
Addition chelating agent and again cooling processing are more conducive to the progress of reaction, carry out squeezing into plasticising when temperature is less than 80 degree
Agent, retarder and remaining styrene, which are diluted, stirs the progress for being more conducive to reaction so as to improve the tensile strength of product
Height, bending strength is good, bus hardness is strong.
In summary, the invention has the advantages that：Toughness is not only increased, cost is also significantly reduced, improves
Tensile strength is high, bending strength and bus hardness.
Embodiment
Embodiment 1, formula：A kind of mold pressing resin, mainly it is made up of the raw material of following quality：Diethylene glycol (DEG) 19.4Kg, phthalic anhydride
7Kg, cis-butenedioic anhydride 27.5Kg, neopentyl glycol 13.8Kg, styrene 25Kg, arene nitro compound polymerization inhibitor 0.009Kg, antioxidant
0.01Kg, copper naphthenate 0.003Kg, plasticizer 0.025Kg, amino carboxylic acid 2Kg.
Wherein, the component proportion of plasticizer is：Fatty acid methyl ester 10Kg；Epoxy aliphatic acid methyl ester 20Kg；Benzoic acid 5Kg；
Activated carbon 1.4Kg；The 4Kg of phosphinylidyne two；Soluble polyvinyl alcohol 5Kg；Epoxidized soybean oil 2Kg；Ethylene glycol 5Kg；Isononyl alcohol 5Kg；Oxidation
Magnesium 0.4Kg；Chlorinated paraffin 15Kg；Epoxy palm oil 4Kg；Roseolic acid 3Kg.
The preparation method of plasticizer is, by fatty acid methyl ester；Epoxy aliphatic acid methyl ester；Benzoic acid；Activated carbon；Phosphinylidyne two；
Soluble polyvinyl alcohol；Epoxidized soybean oil；Ethylene glycol；Isononyl alcohol is stirred in reactor, and reaction temperature is 60-180 DEG C, instead
It is 4 hours between seasonable, then adds magnesia；Chlorinated paraffin；Epoxy palm oil and roseolic acid exist by the intermediate product
180 DEG C~260 DEG C, reacted under conditions of 5Pa~200Pa, obtain plasticizer, take plasticizer 0.025Kg wherein, antioxidant
Component proportion be：Zinc dibutyl dithiocarbamate 0.1Kg；Amino-pyrazol 0.01Kg；Acetyl acetone 0.01Kg；Hydroxyl
Benzophenone 0.01Kg；Loop coil ethylene glycol 0.01Kg；Polyolefine powder 98Kg.
The preparation method of antioxidant is：According to the above ratio by zinc dibutyl dithiocarbamate；Amino-pyrazol；Levulinic
Ketone closes；Loop coil ethylene glycol；Reacted in polyolefine powder input reactor, under the protection of nitrogen, be warming up to 60-80 DEG C,
After adding dihydroxy benaophenonel, reflux state is continuously heating to, after reacting 10-12 hours, 10 DEG C is naturally cooled to, is produced
Product, take antioxidant 0.01Kg.
The preparation method of mold pressing resin：
A) by diethylene glycol (DEG), phthalic anhydride, cis-butenedioic anhydride, diethylene glycol, neopentyl glycol；Polyolefine powder and 2/3 chelating agent are put into successively
In reactor, reaction is started to warm up, when kettle temperature reaches 120 DEG C, starts to stir；
B) under conditions of nitrogen flow is 6m3/h, control and evaporate 100 DEG C of a temperature, after insulation reaction 1h, react voluntarily heat release extremely
140 DEG C, 180 DEG C are warming up to 18 DEG C/h speed, then 190 DEG C are warming up to 4 DEG C/h speed, finally with 9 DEG C/h speed
It is warming up to 200 DEG C；Insulation reaction 3 hours under the conditions of 200 DEG C, react to acid number and reach 60mgKOH/g, by nitrogen flow adjust to
60m3/h, react to acid number and reach 40mgKOH/g；
C) adjust to void tower, nitrogen flow and increase to 85m/h, react to acid number 28mKOH/g, nitrogen flow is adjusted to 10m3/
H, cooling, when temperature of charge is down to 180 DEG C, polymerization inhibitor is added, 170 DEG C is down to and obtains mold pressing resin；
D) add remaining amino carboxylic acid and carry out cooling dilution, when temperature of charge is down to 175 DEG C, start dilution and with per hour 5
DEG C speed carry out being cooled to 80 DEG C；
E) under conditions of temperature is less than 80 DEG C, dilution kettle squeezes into plasticizer, copper naphthenate and styrene in advance, stirs
More than 30min.
Embodiment 2：Formula：A kind of mold pressing resin, mainly it is made up of the raw material of following mass percent：Diethylene glycol (DEG) 20Kg,
Phthalic anhydride 7.6Kg, cis-butenedioic anhydride 28.5Kg, neopentyl glycol 14.5Kg, styrene 30Kg, arene nitro compound polymerization inhibitor 0.009Kg, resist
Oxygen agent 0.015Kg, copper naphthenate 0.031Kg, plasticizer 0.028Kg, amino carboxylic acid 5Kg.
Wherein, the component proportion of plasticizer is：Fatty acid methyl ester 20Kg；Epoxy aliphatic acid methyl ester 30Kg；Benzoic acid 8Kg；
Activated carbon 1.6Kg；The 5Kg of phosphinylidyne two；Soluble polyvinyl alcohol 8Kg；Epoxidized soybean oil 6Kg；Ethylene glycol 10Kg；Isononyl alcohol 10Kg；Oxygen
Change magnesium 0.6Kg；Chlorinated paraffin 20Kg；Epoxy palm oil 10Kg；Roseolic acid 6Kg.
The preparation method of plasticizer is, by fatty acid methyl ester；Epoxy aliphatic acid methyl ester；Benzoic acid；Activated carbon；Phosphinylidyne two；
Soluble polyvinyl alcohol；Epoxidized soybean oil；Ethylene glycol；Isononyl alcohol is stirred in reactor, and reaction temperature is 60-180 DEG C, instead
It is 4 hours between seasonable, then adds magnesia；Chlorinated paraffin；Epoxy palm oil and roseolic acid exist by the intermediate product
180 DEG C~260 DEG C, reacted under conditions of 5Pa~200Pa, obtain plasticizer, take plasticizer 0.028Kg.
Wherein, the component proportion of antioxidant is：Zinc dibutyl dithiocarbamate 0.3Kg；Amino-pyrazol 0.06Kg；Second
Acyl acetone closes 0.02Kg；Dihydroxy benaophenonel 0.02Kg；Loop coil ethylene glycol 0.02Kg；Polyolefine powder 98Kg.
The preparation method of antioxidant is：According to the above ratio by zinc dibutyl dithiocarbamate；Amino-pyrazol；Levulinic
Ketone closes；Loop coil ethylene glycol；Reacted in polyolefine powder input reactor, under the protection of nitrogen, be warming up to 60-80 DEG C,
After adding dihydroxy benaophenonel, reflux state is continuously heating to, after reacting 10-12 hours, 10 DEG C is naturally cooled to, is produced
Product, take antioxidant 0.028Kg.
The preparation method of mold pressing resin：
A) by diethylene glycol (DEG), phthalic anhydride, cis-butenedioic anhydride, diethylene glycol, neopentyl glycol；Polyolefine powder and 2/3 chelating agent are put into successively
In reactor, reaction is started to warm up, when kettle temperature reaches 120 DEG C, starts to stir；
B) under conditions of nitrogen flow is 10m3/h, control and evaporate 105 DEG C of a temperature, after insulation reaction 1.5h, reaction is voluntarily put
Heat is warming up to 180 DEG C to 140 DEG C with 20 DEG C/h speed, then is warming up to 190 DEG C with 5 DEG C/h speed, finally with 10 DEG C/h's
Speed is warming up to 200 DEG C；Insulation reaction 5.5 hours under the conditions of 200 DEG C, react to acid number and reach 70mgKOH/g, by nitrogen flow
Adjust to 80m3/h, react to acid number and reach 45mgKOH/g；
C) adjust to void tower, nitrogen flow and increase to 90m/h, react to acid number 37mKOH/g, nitrogen flow is adjusted to 15m3/
H, cooling, when temperature of charge is down to 180 DEG C, polymerization inhibitor is added, 175 DEG C is down to and obtains mold pressing resin；
D) add remaining amino carboxylic acid and carry out cooling dilution, when temperature of charge is down to 175 DEG C, start dilution and with per hour 10
DEG C speed carry out being cooled to 80 DEG C；
E) under conditions of temperature is less than 80 DEG C, dilution kettle squeezes into plasticizer, copper naphthenate and remaining styrene in advance, stirs
Mix more than 30min.
Embodiment 3：Formula：A kind of mold pressing resin, mainly it is made up of the raw material of following mass percent：Diethylene glycol (DEG)
19.8Kg, phthalic anhydride 7.3Kg, cis-butenedioic anhydride 28Kg, neopentyl glycol 14Kg, styrene 28Kg, arene nitro compound polymerization inhibitor
0.009Kg, antioxidant 0.01Kg, copper naphthenate 0.003Kg, plasticizer 0.026Kg, amino carboxylic acid 3Kg.
Wherein, the component proportion of plasticizer is：Fatty acid methyl ester 15Kg；Epoxy aliphatic acid methyl ester 25Kg；Benzoic acid 6Kg；
Activated carbon 1.5Kg；The 4.5Kg of phosphinylidyne two；Soluble polyvinyl alcohol 6Kg；Epoxidized soybean oil 4Kg；Ethylene glycol 8Kg；Isononyl alcohol 6Kg；Oxygen
Change magnesium 0.5Kg；Chlorinated paraffin 18Kg；Epoxy palm oil 6Kg；Roseolic acid 5Kg.
The preparation method of plasticizer is, by fatty acid methyl ester；Epoxy aliphatic acid methyl ester；Benzoic acid；Activated carbon；Phosphinylidyne two；
Soluble polyvinyl alcohol；Epoxidized soybean oil；Ethylene glycol；Isononyl alcohol is stirred in reactor, and reaction temperature is 60-180 DEG C, instead
It is 4 hours between seasonable, then adds magnesia；Chlorinated paraffin；Epoxy palm oil and roseolic acid exist by the intermediate product
180 DEG C~260 DEG C, reacted under conditions of 5Pa~200Pa, obtain plasticizer, take plasticizer 0.026Kg.
Wherein, the component proportion of antioxidant is：Zinc dibutyl dithiocarbamate 0.2Kg；Amino-pyrazol 0.04Kg；Second
Acyl acetone closes 0.01Kg；Dihydroxy benaophenonel 0.015Kg；Loop coil ethylene glycol 0.015Kg；Polyolefine powder 98Kg.
The preparation method of antioxidant is：According to the above ratio by zinc dibutyl dithiocarbamate；Amino-pyrazol；Levulinic
Ketone closes；Loop coil ethylene glycol；Reacted in polyolefine powder input reactor, under the protection of nitrogen, be warming up to 60-80 DEG C,
After adding dihydroxy benaophenonel, reflux state is continuously heating to, after reacting 10-12 hours, 10 DEG C is naturally cooled to, is produced
Product, take antioxidant 0.01Kg.
The preparation method of mold pressing resin：
A) by diethylene glycol (DEG), phthalic anhydride, cis-butenedioic anhydride, diethylene glycol, neopentyl glycol；Polyolefine powder and 2/3 chelating agent are put into successively
In reactor, reaction is started to warm up, when kettle temperature reaches 120 DEG C, starts to stir；
B) under conditions of nitrogen flow is 8m3/h, control and evaporate 103 DEG C of a temperature, after insulation reaction 1.2h, react voluntarily heat release
To 140 DEG C, 180 DEG C are warming up to 19 DEG C/h speed, then 190 DEG C are warming up to 4.5 DEG C/h speed, finally with 9.5 DEG C/h
Speed be warming up to 200 DEG C；Insulation reaction 4 hours under the conditions of 200 DEG C, react to acid number and reach 65mgKOH/g, by nitrogen flow
Adjust to 70m3/h, react to acid number and reach 43mgKOH/g；
C) adjust to void tower, nitrogen flow and increase to 90m/h, react to acid number 33mKOH/g, nitrogen flow is adjusted to 12m3/
H, cooling, when temperature of charge is down to 180 DEG C, polymerization inhibitor is added, 172 DEG C is down to and obtains mold pressing resin；
D) add remaining amino carboxylic acid and carry out cooling dilution, when temperature of charge is down to 175 DEG C, start dilution and with per hour 7
DEG C speed carry out being cooled to 80 DEG C；
E) under conditions of temperature is less than 80 DEG C, dilution kettle squeezes into plasticizer, copper naphthenate and styrene in advance, stirs
More than 30min.
Embodiment 4：Formula：A kind of mold pressing resin, mainly it is made up of the raw material of following mass percent：Diethylene glycol (DEG)
19.8Kg, phthalic anhydride 7.3Kg, cis-butenedioic anhydride 28Kg, neopentyl glycol 14Kg, styrene 28Kg, arene nitro compound polymerization inhibitor
0.009Kg, antioxidant 0.01Kg, copper naphthenate 0.003Kg, plasticizer 0.026Kg, amino carboxylic acid 3Kg.
In the embodiment, polymerization inhibitor is hydroquinones, and antioxidant is triphenyl phosphite, and retarder is copper naphthenate.
The preparation method of mold pressing resin：
A) by diethylene glycol (DEG), phthalic anhydride, cis-butenedioic anhydride, diethylene glycol, neopentyl glycol；Polyolefine powder and 2/3 chelating agent are put into successively
In reactor, reaction is started to warm up, when kettle temperature reaches 120 DEG C, starts to stir；
B) under conditions of nitrogen flow is 8m3/h, control and evaporate 103 DEG C of a temperature, after insulation reaction 1.2h, react voluntarily heat release
To 140 DEG C, 180 DEG C are warming up to 19 DEG C/h speed, then 190 DEG C are warming up to 4.5 DEG C/h speed, finally with 9.5 DEG C/h
Speed be warming up to 200 DEG C；Insulation reaction 4 hours under the conditions of 200 DEG C, react to acid number and reach 65mgKOH/g, by nitrogen flow
Adjust to 70m3/h, react to acid number and reach 43mgKOH/g；
C) adjust to void tower, nitrogen flow and increase to 90m/h, react to acid number 33mKOH/g, nitrogen flow is adjusted to 12m3/
H, cooling, when temperature of charge is down to 180 DEG C, polymerization inhibitor is added, 172 DEG C is down to and obtains mold pressing resin；
D) add remaining amino carboxylic acid and carry out cooling dilution, when temperature of charge is down to 175 DEG C, start dilution and with per hour 7
DEG C speed carry out being cooled to 80 DEG C；
E) under conditions of temperature is less than 80 DEG C, dilution kettle squeezes into plasticizer, copper naphthenate and styrene in advance, stirs
More than 30min.
Comparative example 1, a kind of mold pressing resin are mainly made up of following Kg raw material：Phthalic anhydride 120Kg, propane diols 290KgKg, it is suitable
Acid anhydride 440Kg, DPG 70Kg, methyl propanediol 40Kg, neopentyl glycol 70Kg, styrene 420Kg.
Comparative example 2, a kind of mold pressing resin are mainly made up of following middle Kg raw material：Phthalic anhydride 130Kg, propane diols 330Kg, it is suitable
Acid anhydride 450Kg, DPG 95Kg, methyl propanediol 45Kg, neopentyl glycol 80Kg, styrene 450Kg.
Embodiment 1-4 performance test with reference to sample performance test with contrasting
It can be drawn by embodiment one to example IV and the testing result of comparative example one and comparative example two, the reality in the present invention
National standard can not only be met by applying the thick shape degree of example one to example IV, and better than comparative example one and comparative example two is thick
Shape degree.Importantly, embodiment one to the tensile strength of example IV, bending strength and bus hardness much compares ratio
Example one and comparative example two it is much higher, so effectively expanding the use range of this kind of mold pressing resin.
This specific embodiment is only explanation of the invention, and it is not limitation of the present invention, people in the art
Member can make the modification of no creative contribution to the present embodiment as needed after this specification is read, but as long as at this
All protected in the right of invention by Patent Law.
Claims (10)
- A kind of 1. mold pressing resin, it is characterised in that：Mainly it is made up of the raw material of following mass percent：Diethylene glycol (DEG) 19.4-20, benzene Acid anhydride 7-7.6, cis-butenedioic anhydride 27.5-28.5, neopentyl glycol 13.8-14.5, styrene 25-30, polymerization inhibitor 0.009, antioxidant 0.01- 0.015, retarder 0.003-0.031, plasticizer 0.025-0.028, chelating agent 2-5.
- 2. mold pressing resin according to claim 1, it is characterised in that：The resin is mainly by the raw material of following mass percent It is made：Diethylene glycol (DEG) 19.7, phthalic anhydride 7.5, cis-butenedioic anhydride 27, neopentyl glycol 14, styrene 31.5, polymerization inhibitor 0.009, antioxidant 0.01, Retarder 0.003, plasticizer 0.025, chelating agent 2.
- 3. mold pressing resin according to claim 1, it is characterised in that：Described antioxidant is mainly by following mass percent Raw material composition：Zinc dibutyl dithiocarbamate 0.1-0.3；Amino-pyrazol 0.01-0.06；Acetyl acetone 0.01- 0.02；Dihydroxy benaophenonel 0.01-0.02；Loop coil ethylene glycol 0.01-0.02；Polyolefine powder 99-99.6.
- 4. mold pressing resin according to claim 1, it is characterised in that：Described plasticizer by following mass percent into It is grouped into：Fatty acid methyl ester 10-20；Epoxy aliphatic acid methyl ester 20-30；Benzoic acid 5-8；Activated carbon 1.4-1.6；The 4-5 of phosphinylidyne two； Soluble polyvinyl alcohol 5-8；Epoxidized soybean oil 2-6；Ethylene glycol 5-10；Isononyl alcohol 5-10；Magnesia 0.4-0.6；Chlorinated paraffin 15- 20；Epoxy palm oil 4-10, roseolic acid 3-6.
- 5. mold pressing resin according to claim 1, it is characterised in that：Described polymerization inhibitor inhibits for arene nitro compound Agent.
- 6. mold pressing resin according to claim 1, it is characterised in that：Described retarder is copper naphthenate.
- 7. mold pressing resin according to claim 1, it is characterised in that：Described chelating agent is amino carboxylic acid or 1,3- diketone One kind.
- 8. for a kind of preparation method of the mold pressing resin described in claim 1, it is characterised in that：Comprise the following steps：A) diethylene glycol (DEG), phthalic anhydride, cis-butenedioic anhydride, diethylene glycol, neopentyl glycol, antioxidant and 2/3 chelating agent are put into reaction successively In kettle, reaction is started to warm up, when kettle temperature reaches 120-140 DEG C, starts to stir；b）Under conditions of nitrogen flow is 6~10m3/h, controls and evaporate 100-105 DEG C of a temperature, after 1~1.5h of insulation reaction, Voluntarily heat release to 140 DEG C, is warming up to 180 DEG C, then be warming up to 190 with 4~5 DEG C/h speed with 18~20 DEG C/h speed for reaction DEG C, finally it is warming up to 200 DEG C with 9~10 DEG C/h speed；c）Adjust to void tower, nitrogen flow and increase to 85-90m/h, react to acid number 28-37mKOH/g, nitrogen flow is adjusted To 10~15m3/h, cooling, when temperature of charge is down to 180 DEG C, polymerization inhibitor is added, be down to 170~175 DEG C and obtain molding tree Fat；d）Add remaining chelating agent and carry out cooling dilution, carry out being cooled to 80 DEG C;e）Under conditions of temperature is less than 80 DEG C, dilution kettle squeezes into plasticizer, retarder and styrene in advance, stirs 30min More than.
- 9. the preparation method of mold pressing resin according to claim 7, it is characterised in that：Step b）It is additionally included in 200 DEG C of bars Insulation reaction 3~5.5 hours under part, react to acid number up to 60~70mgKOH/g, nitrogen flow adjusted to 60~80m3/h, Reaction is to acid number up to 40~45mgKOH/g.
- 10. the preparation method of mold pressing resin according to claim 7, it is characterised in that：In step d）In, first material is dropped After temperature is diluted to 175 DEG C, carry out being cooled to 80 DEG C with 5-10 DEG C per hour of speed.
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| CN201610548076.7A CN107603116A (en) | 2016-07-12 | 2016-07-12 | Mold pressing resin and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109575256A (en) * | 2018-12-04 | 2019-04-05 | 镇江利德尔复合材料有限公司 | A kind of raising outdoor electric appliance insulation performance and the mold pressing resin of heat distortion temperature and preparation method thereof |
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Application publication date: 20180119 |