CN1099043A - Produce resol and moulding compound thereof with starch - Google Patents

Produce resol and moulding compound thereof with starch Download PDF

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Publication number
CN1099043A
CN1099043A CN 94101980 CN94101980A CN1099043A CN 1099043 A CN1099043 A CN 1099043A CN 94101980 CN94101980 CN 94101980 CN 94101980 A CN94101980 A CN 94101980A CN 1099043 A CN1099043 A CN 1099043A
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China
Prior art keywords
starch
resol
moulding compound
phenol
resin
Prior art date
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Pending
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CN 94101980
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Chinese (zh)
Inventor
陈国民
李林远
顾星若
张翔
许永飞
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Xi'an Xinhui Science And Tech Industrial Co No43 Inst Astronautic Industrial
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Xi'an Xinhui Science And Tech Industrial Co No43 Inst Astronautic Industrial
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Priority to CN 94101980 priority Critical patent/CN1099043A/en
Publication of CN1099043A publication Critical patent/CN1099043A/en
Pending legal-status Critical Current

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Abstract

The invention belongs to resol and moulding compound material thereof.With widely distributed inexpensive Ipomoea batatas (cassava, konjaku, potato) starch as main component single stage method synthesizing new resol, be equipped with filler and other Synergist S-421 95 is made moulding compound.This material all adopts traditional processing method preparation.The phenol waste liquid adopts novel refrigerated separation method to carry out intermediate treatment, and technology is simple, rate of recovery height.This material technology index all satisfies or is better than specified requirement, and production cost is low, and economic benefit and obvious social benefit can be widely used in national economy every field such as machinery, electrical equipment, instrument, daily necessities.

Description

Produce resol and moulding compound thereof with starch
The present invention relates to the manufacturing technology field of a kind of resol and moulding compound material thereof, it is with starch in replace formaldehyde and part phenol and make.
In prior art, industrial thermoplasticity phenol-formaldehyde resin is to react under an acidic catalyst effect with phenol and formaldehyde to form, and it is equipped with filler again and moulding compound is processed in other partition agent.Comparing its defective with starch is 1) formaldehyde price height, transportation and bunkerage complexity and expense height.2) formaldehyde enters in the waste liquid, contaminate environment, and liquid waste disposal difficulty, expenses of environmental protection are big.3) behind operator's suction or the skin absorption formaldehyde, meeting exciting eye, skin and respiratory tract suppress central nervous system, cause anesthesia, certainly will cause strict labour protection, increase labor insurance fees usefulness.According to document announcement, the research of resol and molding powder thereof was once carried out producing with W-Gum in the North America, document is " Corn Starch:a low-cost roure to novolac resin " mod Plast, 1980, and 57(2) 69.74(Eng).But do not see the report of its industrializing implementation so far.It is technical to have tangible limitation, and weak point is: one only is a Semen Maydis powder, and the price comparison height; Its two, the moulding compound prescription has only a trade mark, resol, hexamethylenetetramine content height, the product cost height is used no specific aim; Its three, the processing of not mentioned waste liquid.
The objective of the invention is to avoid the above defective of the prior art or weak point to propose a kind of practicable technological approaches of producing resol and moulding compound thereof with starch.
Purpose content of the present invention can reach by following measure, and the direct single step reaction of heated and stirred under the catalyst sulfuric acid effect gets with the sodium hydroxide neutralization to suitable molecular weight resol by phenol and Ipomoea batatas (cassava, konjaku, potato) starch; Its formula range (wt0/0) is: phenol 45.0-55.0, sulfuric acid 0.4.0.7, Ipomoea batatas (cassava, konjaku, potato) starch 45.0-55.0, sodium hydroxide 0.2-0.3 and water 2.2-2.3.Moulding compound is equipped with filler by resol and other partition agent adopts traditional roll-in method to process;
Its formula range (wt0/0) is a table 1
Figure 941019802_IMG1
With the refrigerated separation method high concentration phenol liquid waste disposal that produces is become lower concentration phenol waste liquid, directly recycling overwhelming majority phenol.
The present invention has compared following advantage with present technology.
1. starting material are extensive, and selectivity is good, and is cheap, and product cost is low.
2. moulding compound is used pointed.
3. simple liquid waste disposal, can add directly and utilize 90% phenol again, environmental pollution is little, and expenses of environmental protection is low.
The surface description of subordinate list is as follows:
1. the ratio range table of phenol-starch phenolaldehyde moulding compound
2. formula table is surveyed in the enforcement of phenol-starch phenolaldehyde moulding compound
3. the technical indicator table of phenol-starch resol
4. the technical indicator table of phenol-starch phenolaldehyde moulding compound
Most preferred embodiment of the present invention is:
The synthetic best prescription (wt0/0) of implementing of resol is:
Phenol 46.4, sulfuric acid 0.6, Ipomoea batatas (cassava, konjaku, potato) starch 50.4, sodium hydroxide 0.3 and water 2.3.Be ready to raw material by prescription, one time charging capacity should not make reactor coefficient>0.7.Phenol, Ipomoea batatas (cassava, konjaku, potato) starch and sulfuric acid input are added a layer reactor, heat up and stir.When temperature reached 105 ℃ of left and right sides, starch began gelation, stopped this moment stirring.Treat to heat up again after the basic hydrolysis of starch and stir, be warmed up to 180 ± 5 ℃ always, the insulation polycondensation, reaction times>2H, reactant viscosity with vacuum tightness 0.04~0.05mpa, vacuumizes the dehydration polycondensation, dewatering time>20min near after requiring.After reaching viscosity, remove vacuum, be cooled to about 130 ℃, use in the sodium hydroxide and resin, blowing afterreaction still gets finished product.Its technical indicator such as table 3:
Figure 941019802_IMG2
Moulding compound is made the best prescription (wt%) of implementing as table 2:
Figure 941019802_IMG3
The starting material that need are pulverized are through the crusher coarse crushing, and Universalpulverizer is in small, broken bits to fineness requirement, gets all the each component ready by prescription, and in certain sequence material is added in the mixing machine, each 〉=60min between being mixed into.Twin-roll machine working roll temperature is raised to 100~110 ℃, and the idle roll temperature is raised to 140~150 ℃, and dancer rools is 3.0~4.0mm, with the speed that is fit to compound is added in the twin-roll machine, and the heat refining suitable time gets sheet stock substantially uniformly.After the sheet stock cooling, through the crusher coarse crushing, Universalpulverizer is in small, broken bits to fineness requirement.Need through magnetic separation after sheet stock is in small, broken bits.With different order of classes or grades at school, the moulding compound after the magnetic separation is pieced together batch mixing and is closed 45min, and metering packing gets product, its technical indicator such as table 4.
Figure 941019802_IMG4
* make red-hot rod leave test specimen behind the 3min, the sample X visible flame that do not have in 30S.
Make red-hot rod leave test specimen behind the △ 3min, in 1ls, do not have visible flame on the sample.
The waste liquid cooling process: with reactor distilled high concentration phenol waste liquid through apparatus for supercooling be cooled to~-2 ℃, the phenol crystallization is separated out.Leave standstill and allow the solid-liquid layering, time of repose>2h pours out liquid portion and gets crystalline phenol, and directly utilizes again, and the phenol recovery rate can reach 90%.

Claims (3)

1, a kind ofly produces resol and moulding compound thereof, it is characterized in that resol moiety (wt%) is: phenol 45.0~55.0, sulfuric acid 0.4~0.7, Ipomoea batatas (cassava, evil spirit in, potato) starch 45.0~55.0, sodium hydroxide 0.2~0.3 and water 2.2~2.3 with starch; Moulding compound moiety (wt%) is:
Trade mark PF2A1, resin 35.0~40.0, wood powder 40.0~50.0, hexamethylenetetramine 4.0~8.0, magnesium oxide 0.6, calcium sulfate 4.0~9.0, Zinic stearas 1.0 and glossy black 1.0;
Trade mark PF2A2, resin 40.0~45.0, wood powder 45.0~50.0, hexamethylenetetramine 5.0~9.0, magnesium oxide 0.8, calcium sulfate 3.0~8.0, Zinic stearas 1.0 and glossy black 1.0;
Trade mark PF2C4, resin 35.0~40.0, wood powder 30.0~35.0, hexamethylenetetramine 4.0~8.0, magnesium oxide 0.6, calcium sulfate 20.0~25.0, Zinic stearas 1.0 and glossy black 1.0.]
2, according to claim 1 with starch resol and moulding compound thereof, it is characterized in that the optimum formula (wt%) of resol is: phenol 46.4, sulphur join 0.6, Ipomoea batatas (cassava, konjaku, potato) starch 50.4, sodium hydroxide 0.3 and water 2.3; The optimum formula of moulding compound (wt%) is:
Trade mark PF2A1, resin 37.0, wood powder 48.0, hexamethylenetetramine 5.5, magnesium oxide 0.6, calcium sulfate 6.9, Zinic stearas 1.0 and glossy black 1.0;
Trade mark PF2A2, resin 40.5, wood powder 46.0, hexamethylenetetramine 6.1, magnesium oxide 0.8, calcium sulfate 4.6, Zinic stearas 1.0 and glossy black 1.0;
Trade mark PF2C4, resin 37.0, wood powder 32.0, hexamethylenetetramine 5.5, magnesium oxide 0.6, calcium sulfate 22.9, Zinic stearas 1.0 and glossy black 1.0.
3, according to claim 1,2 described with starch resol and moulding compounds thereof, the waste liquid cooling treatment method is characterized in that phenol waste liquid temperature~-2 ℃, and time of repose>2h returns the phenol that the liquid separation obtains recovery.
CN 94101980 1994-02-23 1994-02-23 Produce resol and moulding compound thereof with starch Pending CN1099043A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 94101980 CN1099043A (en) 1994-02-23 1994-02-23 Produce resol and moulding compound thereof with starch

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Application Number Priority Date Filing Date Title
CN 94101980 CN1099043A (en) 1994-02-23 1994-02-23 Produce resol and moulding compound thereof with starch

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CN1099043A true CN1099043A (en) 1995-02-22

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CN 94101980 Pending CN1099043A (en) 1994-02-23 1994-02-23 Produce resol and moulding compound thereof with starch

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101200528B (en) * 2007-12-04 2010-06-16 中国林业科学研究院木材工业研究所 Method for preparing formaldehyde-phenol resin by using starch
CN101182368B (en) * 2007-12-11 2010-11-03 武汉理工大学 Method for synthesizing high-molecular-weight thermoplastic phenol resin
CN106854263A (en) * 2016-12-11 2017-06-16 钦州学院 A kind of starch conversion phenolic resin and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101200528B (en) * 2007-12-04 2010-06-16 中国林业科学研究院木材工业研究所 Method for preparing formaldehyde-phenol resin by using starch
CN101182368B (en) * 2007-12-11 2010-11-03 武汉理工大学 Method for synthesizing high-molecular-weight thermoplastic phenol resin
CN106854263A (en) * 2016-12-11 2017-06-16 钦州学院 A kind of starch conversion phenolic resin and preparation method thereof

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