CN1240806A - Process for preparing phenolaldehyde moulding compound - Google Patents

Process for preparing phenolaldehyde moulding compound Download PDF

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Publication number
CN1240806A
CN1240806A CN 98112125 CN98112125A CN1240806A CN 1240806 A CN1240806 A CN 1240806A CN 98112125 CN98112125 CN 98112125 CN 98112125 A CN98112125 A CN 98112125A CN 1240806 A CN1240806 A CN 1240806A
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China
Prior art keywords
moulding compound
agent
wollastonite
toughener
consumption
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CN 98112125
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CN1105143C (en
Inventor
周琨生
傅旭
刘彬
胡卫东
李军
王进
兰修才
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CHENGUANG CHEMICAL RESEARCH ACADEMY (CHENGDU) MINISTRY OF CHEMICAL INDUSTRY
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CHENGUANG CHEMICAL RESEARCH ACADEMY (CHENGDU) MINISTRY OF CHEMICAL INDUSTRY
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Priority to CN98112125A priority Critical patent/CN1105143C/en
Publication of CN1240806A publication Critical patent/CN1240806A/en
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Abstract

A process for preparing phenolaldehyde moulding material uses such raw materials as phenolic resin, wallastonite or the composite of wallastonite and glass fibre as reinforcing agent, the aqueous solution of hexamethylenetetramine as solidifying agent, silane as coupling agent and demoulding agent, and includes pulverizing and rolling. Its advantages are simple process, improved operating environment, high temp. and insulating nature of the moulding material, and easy shaping.

Description

The preparation method of phenolaldehyde moulding compound
The present invention is a kind of preparation method of phenolaldehyde moulding compound, comprises moulding compound is processed into goods, belongs to polymeric material field.
Phenolaldehyde moulding compound is widely used in industrial circles such as electronic apparatus.In the prior art, the composition of phenolaldehyde moulding compound mainly contains: resin, filler, solidifying agent, lubricant and tinting material etc., wherein filler is mainly wood powder, asbestos, talcum powder, mica powder, silica powder, glass cloth or silk etc.Many based on single filler in the prescription, though be that the moulding compound toughness and the intensity of filler preparation is better with wood powder or asbestos, visual appearance is poor, and is mobile not good enough, can't the high-accuracy product of moulding; Though with talcum powder, mica powder or silica powder is that moulding compound rigidity, the outward appearance of filler preparation is good, fragility is big.Both just constituted compounded mix, also be difficult to overcome above-mentioned defective with wood powder etc.Making filler (or toughener) with woven fiber glass only can prepared layer pressing plate or the simple thin-wall part of profile; Make filler with the glass bundle and can cause defectives such as goods orientation and skewness.
The preparation technology of phenolaldehyde moulding compound mainly contains two big classes: dry method and wet method.Dry method comprises roll-in method and screw extrusion method; Wet method comprises solution method, water miscible liquid method and resin raw material pickling process.In these methods, the most simple and easy to do with roll-in method.Concrete operations are: raw material pulverizing---mixes---roll-in---pulverizing---moulding compound.Wherein the fineness degree of solidifying agent is very big to the quality product influence, generally is more better, will reach 120 orders at least.But the easy moisture absorption of solidifying agent hexamethylenetetramine, and dust is bigger when pulverize separating, and operational condition is abominable.
The objective of the invention is to prepare the phenolaldehyde moulding compound of a kind of intensity height, good toughness, high temperature resistant, good insulating, easy-formation.
The object of the present invention is achieved like this: formed through pulverizing roll-in by pheno-ether resin, toughener, solidifying agent, it is characterized in that: (a) toughener is the mixture of wollastonite or wollastonite and glass fibre, wherein the wollastonite consumption is 55~78%, and the glass fibre consumption is 0~15%; (b) solidifying agent is the hexamethylenetetramine aqueous solution, and wherein the consumption of solidifying agent is 1.5~2%, and solidifying agent and water are by 1: 1~2 mixed dissolutions; (c) the pheno-ether resin consumption is 20~27%; (d) pheno-ether resin and wollastonite, the aqueous solution of curing agent after will pulverizing mixes, 60~70 ℃ dry 6~8 hours down, on the roller temperature is 110~130 ℃ roll squeezer, mix then, cool off, pulverize moulding compound.
This moulding compound can be with moulding shaping process or transfer molding technological forming, moulding compound is added after 10~15 minutes in the die cavity 80~100 ℃ of following preheatings, and die temperature is 170~180 ℃, and pressure is 40~15MPa, molding time is 3~5 minutes/mm, promptly gets goods.
Wherein, also can add 0.7% silane coupling agent in the moulding compound, 0~0.6% releasing agent.
During the preparation moulding compound, at first intoxicated ether resin is pulverized, fineness reaches 30 orders and gets final product.Wollastonite is 800~1000 orders.About 5~7 μ of glass fiber diameter, length all can greater than 0.2mm or continuous long glass fiber.Then resin, wollastonite, aqueous solution of curing agent are mixed in homogenizer, 60~70 ℃ were dried by the fire 6~8 hours down, remove moisture content.
Be roll-in on 110~130 ℃ the twin-roll machine with dried material, add glass fibre by proportioning simultaneously, after the roll-in evenly, get final product slice in the roller temperature, pulverize at last moulding compound.
Accompanying drawing is a process flow sheet of the present invention.
The present invention adopts the roll-in method production technology to prepare moulding compound, owing to adopt curing agent water-soluble Liquid makes curing agent reach refinement degree on the molecular level, has not only reduced the curing agent pulverizing process, Avoid the bigger defective of dust, but also greatly improved properties of product.
When adopting wollastonite and glass fibre compounded mix to be reinforcing agent, can be by adjusting silicon The ratio of lime stone and glass fibre is regulated flowability and the impact flexibility of moulding compound, makes it both In the time of satisfying transfer molding to material fluidity and each to uniform requirement, can satisfy glass again The requirement that strengthens reaches the strong and unyielding purpose of taking into account.
The characteristics such as that the moulding compound of the present invention preparation has is high temperature resistant, insulation, easy-formation can be made The little complex precise spare to 0.2mm of standby wall thickness, mould shrinkage factor 0.3~0.5%, compressive strength>200MPa, heat distortion temperature (1.MPa)>250 ℃ (after processing). Also has good anti-electricity Arc, sheet resistance 〉=1.0 * 1014Ω, volume resistance 〉=1.0 * 1012Ω m, electric Intensity 〉=10MV/m (90 ℃ step by step). Can be widely used in the insulator of air appliance coupling And car electrics aspect.
Be embodiments of the invention below.
Embodiment one:
Get 20 parts of pheno-ether resins (I), 0.6 part of magnesium stearate (II), 2 parts of hexamethylenetetramines (III), 77.4 parts of wollastonites (IV).I is crushed to 30 orders, and III is crushed to 120 orders.Above-mentioned raw materials is mixed, and is roll-in in 120 ± 5 ℃ the twin-screw extruder in the roller temperature, treat that material is mixing to get final product slice after evenly, through cooling, pulverize moulding compound.
Adopt compression molding moulding sample.170 ± 5 ℃ of die plate temperature, pressure 40~80MPa, press time 4min/mm.Test result is: water-intake rate 0.03%, 238.0 ℃ of heat-drawn wires (1.8MPa), compressive strength 200MPa, electrical strength 10.9MV/m, surface resistivity 1.3 * 10 15Ω, volume specific resistance 1.4 * 10 12Ω m.
Embodiment two:
Get I20 part, II0.5 part, III1.5 part, IV78 part.Preparation technology and moulding process are with embodiment one.Test result is: water-absorbent 0.02%, 257.1 ℃ of heat-drawn wires, compressive strength 231MPa, electrical strength 10.5MV/m, surface resistivity 2.9 * 10 15Ω, volume specific resistance 4.6 * 10 22Ω m.
Embodiment three:
Get I27 part, II0.6 part, III2 part, IV70 part, 0.7 part of silane coupling agent (V).III and water by the dissolving that is mixed in 1: 2, are mixed drying with all the other components again.Preparation technology and moulding process are with embodiment one.Test result is: 268.0 ℃ of heat-drawn wires, compressive strength 301MPa, electrical strength 13.7MV/m, surface resistivity 1.3 * 10 14Ω, volume specific resistance 1.8 * 10 13Ω m, shock strength 9.78kJ/m 2
Embodiment four:
Get I27 part, II0.6 part, III2 part, IV55 part, V0.7 part, 15 parts in glass fibre.With III and water by the dissolving that is mixed in 1: 2, again with I, II, IV, V combination drying.By embodiment one technology the good material of drying is carried out mixingly, add simultaneously glass fibre in proportion, mixingly get final product slice, cooling, pulverizing after evenly.Sample forming method and technology are with embodiment one.Test result is: shock strength 13.7kJ/m 2, other performances are identical with embodiment three.
Embodiment five:
Get I28 part, III2 part, IV55 part, 15 parts in glass fibre.III and water by the dissolving that is mixed in 1: 1.5, were stirred for 30 seconds in high speed agitator with I, IV again, and discharging 60 ℃ of bakings 8 hours down, is prepared and moulding by embodiment four technologies then.Test result is: shrinking percentage 0.4%, water-absorbent 0.01%, 263 ℃ of heat-drawn wires (1.8MPa), compressive strength 222MPa, shock strength 13.7kJ/m 2, electrical strength 10.6MV/m, surface resistivity 1.1 * 10 14Ω, volume specific resistance 1.2 * 10 12Ω m.

Claims (3)

1. the preparation method of a phenolaldehyde moulding compound is pulverized roll-in and is formed by pheno-ether resin, toughener, solidifying agent, it is characterized in that:
A. toughener is the mixture of wollastonite or wollastonite and glass fibre, and wherein the wollastonite consumption is 55~78% (weight ratios), and the glass fibre consumption is 0~15% (weight ratio);
B. solidifying agent is the aqueous solution of hexamethylenetetramine, and solidifying agent and water are by 1: 1~2 mixed dissolutions, and hardener dose is 1.5~2% (weight ratios);
C. the pheno-ether resin consumption is 20~27% (weight ratios);
D. the resin after the above-mentioned pulverizing and toughener, aqueous solution of curing agent are mixed, 60~70 ℃ dry 6~8 hours down, on the roller temperature is 110~130 ℃ roll squeezer, mix then, cooling pulverize moulding compound.
2. preparation method according to claim 1 is characterized in that adopting moulding shaping process or transfer molding technological forming, and moulding compound is added in the die cavity behind 80~100 ℃ of following preheating 10~15min.Die temperature is 170~180 ℃, and pressure is 40~150MPa, and molding time is 3~5min/mm, promptly gets product.
3. according to claim 1,2 described preparation methods, it is characterized in that also can adding silane coupling agent 0~0.7% releasing agent 0~0.6%.
CN98112125A 1998-07-06 1998-07-06 Process for preparing phenolaldehyde moulding compound Expired - Fee Related CN1105143C (en)

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CN98112125A CN1105143C (en) 1998-07-06 1998-07-06 Process for preparing phenolaldehyde moulding compound

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Application Number Priority Date Filing Date Title
CN98112125A CN1105143C (en) 1998-07-06 1998-07-06 Process for preparing phenolaldehyde moulding compound

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CN1240806A true CN1240806A (en) 2000-01-12
CN1105143C CN1105143C (en) 2003-04-09

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101974198A (en) * 2010-10-14 2011-02-16 常熟东南塑料有限公司 Heat-resisting phenolic moulding compound
CN105924895A (en) * 2016-06-30 2016-09-07 禹州市远大塑料电器有限责任公司 High-temperature-resistant phenolic moulding plastic
CN107163499A (en) * 2017-07-15 2017-09-15 芜湖乾凯材料科技有限公司 High strength fibre reinforced plastics wall hanging board and preparation method thereof
CN107325481A (en) * 2017-08-16 2017-11-07 常州信息职业技术学院 A kind of phenoplasts inspection shaft well lid and preparation method thereof

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3546157A (en) * 1968-04-25 1970-12-08 Haveg Industries Inc Filled phenolic resin compositions containing a minor amount of a polyolefin
CN1062150A (en) * 1991-12-20 1992-06-24 西北工业大学 Flame-retardant glass fibre reinforced plastic materals
CN1037184C (en) * 1992-06-26 1998-01-28 中国科学院长春应用化学研究所 Preparation of phenolic resin composite material
US5691409A (en) * 1995-07-12 1997-11-25 Sumitomo Bakelite Company Limited Phenolic resin molding material

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101974198A (en) * 2010-10-14 2011-02-16 常熟东南塑料有限公司 Heat-resisting phenolic moulding compound
CN101974198B (en) * 2010-10-14 2012-07-11 常熟东南塑料有限公司 Heat-resisting phenolic moulding compound
CN105924895A (en) * 2016-06-30 2016-09-07 禹州市远大塑料电器有限责任公司 High-temperature-resistant phenolic moulding plastic
CN107163499A (en) * 2017-07-15 2017-09-15 芜湖乾凯材料科技有限公司 High strength fibre reinforced plastics wall hanging board and preparation method thereof
CN107325481A (en) * 2017-08-16 2017-11-07 常州信息职业技术学院 A kind of phenoplasts inspection shaft well lid and preparation method thereof

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