CN103880875B - A kind of preparation method of solid sand coupling agent - Google Patents
A kind of preparation method of solid sand coupling agent Download PDFInfo
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- CN103880875B CN103880875B CN201210552535.0A CN201210552535A CN103880875B CN 103880875 B CN103880875 B CN 103880875B CN 201210552535 A CN201210552535 A CN 201210552535A CN 103880875 B CN103880875 B CN 103880875B
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Abstract
The invention discloses a kind of preparation method of solid sand coupling agent, comprises the following steps：(1) by the rectifying still material input reactor in 3 (2 aminoethyl) aminopropyl alkoxy silane production process, solvent and aminated compounds are added in reactor, control temperature of reaction kettle is at 20～150 DEG C, stirring reaction 1～15 hour, then by reactant separation of solid and liquid, filtrate and amine hydrochlorate sediment are isolated；(2) the filtrate decompression distillation (1) step isolated, the solvent in filtrate are distillated by distilling apparatus, and in reactor, surplus materials as consolidates sand coupling agent；The solvent is C1～C5Straight or branched alkane alcohol, consumption for rectifying still material quality 5%～30%；The aminated compounds is liquefied ammonia, ethylenediamine, diethylenetriamine, triethylene tetraamine, cyclohexylamine, the one kind in aniline, consumption for rectifying still material quality 3%～30%.Solid sand coupling agent prepared by said method can play long-acting stabilization.
Description
Technical field
The present invention relates to a kind of preparation method of solid sand coupling agent, more particularly to utilize 3- (2- aminoethyls)-aminopropyl
The preparation method of the solid sand coupling agent of raw material production based on rectifying still material in alkoxy silane production process.
Background technology
Gu sand coupling agent is applied to casting industry, coupled action can be played to molding sand and resin, improve casting core
Mechanical strength.Before, the solid sand coupling agent that founding materials factory generally adopts has KH-550 (three ethoxy silane of aminopropyl), KH-602
(3- (2- aminoethyls)-aminopropyltriethoxy dimethoxysilane) etc., though above-mentioned solid sand coupling agent can significantly improve adhesion strength,
Use cost is higher.Therefore founding materials factory is more willing to use with same connection effect and cheap coupling agent by-product
Product, therefore just have an opportunity to be able to fast development using rectifying still material deep processed product.
Raw material based on rectifying still material in existing utilization 3- (2- aminoethyls)-aminopropyl alkoxy silane production process
The method of sand coupling agent is consolidated in preparation：Put in 3- (2- aminoethyls)-aminopropyl alkoxy silane production process in reactor
Rectifying still material, then in the reactor the appropriate ratio of blending solvent, solid sand coupling agent product is just obtained after agitation and dilution.
Solid sand coupling agent prepared by said method has the drawback that：Product stability is not good, stores after being added to resin
Failure will be hydrolyzed less than one week, the requirement of low-end market can only be met, lack the market competitiveness.
The content of the invention
It is an object of the invention to provide a kind of production capacity is big, low cost, the preparation method of the simple sand coupling agent admittedly of control, institute
The solid sand coupling agent hydrolysis rate that obtains is stable, and resin compatible it is good, long-acting stable effect can be played.
For achieving the above object, present invention employs technical scheme below.
A kind of preparation method of solid sand coupling agent, with 3- (2- aminoethyls)-aminopropyl alkoxy silane production process
Raw material based on rectifying still material, is characterized in：Step is as follows：(1) 3- (2- aminoethyls)-aminopropyl alkoxy silane was produced
In rectifying still material input reactor in journey, solvent and aminated compounds are added in reactor, temperature of reaction kettle is controlled 20
～150 DEG C, stirring reaction 1～15 hour, then by reactant separation of solid and liquid, isolates filtrate and amine hydrochlorate sediment；⑵
The filtrate decompression distillation that (1) step is isolated, the solvent in filtrate is distillated by distilling apparatus, is remained after distillation in reactor
Excess matter as consolidates sand coupling agent；Above-mentioned solvent is C1～C5Straight or branched alkane alcohol, consumption be rectifying still material quality
5%～30%；Above-mentioned aminated compounds be liquefied ammonia, ethylenediamine, diethylenetriamine, triethylene tetraamine, cyclohexylamine, in aniline
One kind, consumption for rectifying still material quality 3%～30%.
Further, the preparation method of aforesaid a kind of solid sand coupling agent, wherein, described 3- (2- aminoethyls)-ammonia third
Base alkoxy silane is：3- (2- aminoethyls)-aminopropyltriethoxy dimethoxysilane, 3- (2- aminoethyls)-aminopropyl trimethoxy
In base silane, 3- (2- aminoethyls)-aminopropyltriethoxy diethoxy silane, 3- (2- aminoethyls)-aminopropyl triethoxysilane
One or more mixture.
Further, the preparation method of aforesaid a kind of solid sand coupling agent, wherein, step (1) described in solvent be methyl alcohol
Or ethanol.
Further, the preparation method of aforesaid a kind of solid sand coupling agent, wherein, step (1) described in aminated compounds
For diethylenetriamine.
Further, the preparation method of aforesaid a kind of solid sand coupling agent, wherein, the amine hydrochlorate that (1) step is isolated sinks
Starch is ammonium chloride, second di-ammonium salts hydrochlorate, diethylenetriamine hydrochloride, triethylene tetraamine hydrochloride, cyclohexylamine hydrochloride, benzene
One or more in amine hydrochlorate.
Further, the preparation method of aforesaid a kind of solid sand coupling agent, wherein, if the amine salt acid that (1) step is isolated
Ammonium chloride is not contained in salt sediment, then in amine hydrochlorate sediment adds sodium alkoxide, stirring reaction to obtain alcohol, free amine
Compound and sodium chloride, then by reactant separation of solid and liquid, isolate the mixture and chlorine of alcohol and free aminated compounds
Change sodium sediment, Sodium chloride deposit thing obtains solid sodium chloride, alcohol and the free purified separation of amine mixture after drying
It is converted to raw material input step afterwards again（1）In recycle.
Further, the preparation method of aforesaid a kind of solid sand coupling agent, wherein, the sodium alkoxide is preferably liquid methanol
Sodium or liquid ethanol sodium.
Beneficial effects of the present invention：The solid sand coupling agent hydrolysis rate that prepared by the method for the invention is stable, and resin
Compatibility is good, and the resin shelf-life is 1 month, can play long-acting stabilization；The solid sand coupling agent of 1 ton of production can be consumed
1.2 tons or so of 3- (2- aminoethyls)-aminopropyl alkoxy silane rectifying still material, solvent and aminated compounds can be reclaimed and be followed
Ring is utilized, and has the advantages that big production capacity, low cost, control are simple；Founding materials factory is met well to solid sand coupling agent
The requirement of compatibility, pot-life and low cost control.
Heretofore described 3- (2- aminoethyls)-aminopropyl alkoxy silane, may be selected initial feed ethylenediamine: chlorine third
The molar ratio of base silane is（5～15）∶1.
Specific embodiment
It is further described to originally bright below by specific embodiment, but the present invention is not limited in described enforcement
Among example scope.
Embodiment 1.
(1) the rectifying still material 400g of 3- (2- aminoethyls)-aminopropyltriethoxy dimethoxysilane is put in reactor,
40g methyl alcohol, 80g diethylenetriamines are added in reactor, control temperature of reaction kettle at 40～60 DEG C, stirring reaction 8 hours, so
Afterwards by reactant centrifugal filtration, the common 350g of filtrate, the hydrochloride 165g of diethylenetriamine are obtained；(2) the filter (1) step isolated
Solvent under reduced pressure in filtrate is distillated, obtains methyl alcohol 33g by flash column vacuum distillation by liquid, and in reactor, surplus materials is
Gu sand coupling agent, gross weight are 315g；In the diethylenetriamine hydrochloride that (1) step is isolated add 160g mass concentrations
For 28% liquid methanol sodium, stirring reaction displacement, the mixture of methyl alcohol, diethylene triamine and sodium chloride is obtained, was centrifuged
Filter, obtains the common 250g of the mixture of methyl alcohol and diethylene triamine and Sodium chloride deposit thing, and Sodium chloride deposit thing is after drying
It is converted to feedstock circulation utilization after the purified separation of mixture for obtaining solid sodium chloride 73g, methyl alcohol and diethylene triamine again.
Embodiment 2.
(1) the rectifying still material 400g of 3- (2- aminoethyls)-aminopropyltriethoxy diethoxy silane is put in reactor,
120g ethanol, 80g diethylenetriamines are added in reactor, control temperature of reaction kettle at 60～80 DEG C, stirring reaction 3 hours,
Then by reactant centrifugal filtration, the common 332g of filtrate, the hydrochloride 163g of diethylenetriamine are obtained；(2) (1) step is isolated
Solvent under reduced pressure in filtrate is distillated, obtains ethanol 100g by flash column vacuum distillation by filtrate, and in kettle, surplus materials is as solid
Sand coupling agent, gross weight are 318g；(3) in the diethylenetriamine hydrochloride that (1) step is isolated, addition 200g mass concentrations are
18% liquid ethanol sodium, stirring reaction displacement, obtains the mixture of ethanol, diethylene triamine and sodium chloride, centrifugal filtration,
The common 288g of the mixture of ethanol and diethylene triamine and Sodium chloride deposit thing are obtained, Sodium chloride deposit thing is obtained after drying
It is converted to feedstock circulation utilization to after the purified separation of mixture of solid sodium chloride 74g, ethanol and diethylene triamine again.
Embodiment 3.
(1) the rectifying still material 400g of 3- (2- aminoethyls)-aminopropyl trimethoxysilane is put in reactor, to anti-
20g methyl alcohol is added in answering kettle, under stirring condition, 16g liquefied ammonia is passed through in reactor, control temperature of reaction kettle at 20～40 DEG C, stir
Reaction 12 hours is mixed, then by reactant centrifugal filtration, the common 375g of filtrate, ammonium chloride 60g is obtained；(2) (1) step is isolated
Solvent under reduced pressure in filtrate is distillated, obtains methyl alcohol 8g by flash column vacuum distillation by filtrate, and in kettle, surplus materials as consolidates sand
Coupling agent, gross weight is 365g, methyl alcohol reusable edible.
Embodiment 4.
(1) the rectifying still material 400g of 3- (2- aminoethyls)-aminopropyl triethoxysilane is put in reactor, to anti-
30g ethanol is added in answering kettle, under stirring condition, 20g liquefied ammonia is passed through in reactor, control temperature of reaction kettle at 100～120 DEG C,
Stirring reaction 2 hours, then by reactant centrifugal filtration, obtains the common 383g of filtrate, ammonium chloride 65g；(2) (1) step is isolated
Filtrate by flash column vacuum distillation, the solvent under reduced pressure in filtrate is distillated, ethanol 20g is obtained, in kettle, surplus materials is
Gu sand coupling agent, gross weight is 361g, ethanol reusable edible.
Embodiment 5.
(1) by rectifying still material 200g and 3- (2- the aminoethyls)-ammonia third of 3- (2- aminoethyls)-aminopropyl trimethoxysilane
The rectifying still material 200g of ylmethyl dimethoxysilane is put in reactor, and 40g methyl alcohol, stirring condition are added in reactor
It is lower to be passed through 20g liquefied ammonia in reactor, control temperature of reaction kettle at 110～130 DEG C, stirring reaction 2 hours, then by reactant
Centrifugal filtration, obtains the common 380g of filtrate, ammonium chloride 69g；(2) the filtrate (1) step isolated, will by flash column vacuum distillation
Solvent under reduced pressure in filtrate is distillated, and obtains methyl alcohol 23g, surplus materials as admittedly sand coupling agent in kettle, and gross weight is 353g, methyl alcohol
Reusable edible.
Embodiment 6.
(1) by rectifying still material 200g and 3- (2- the aminoethyls)-ammonia third of 3- (2- aminoethyls)-aminopropyl triethoxysilane
The rectifying still material 200g of ylmethyl diethoxy silane is put in reactor, and 35g ethanol, stirring condition are added in reactor
It is lower to be passed through 30g liquefied ammonia in reactor, control temperature of reaction kettle at 130～150 DEG C, stirring reaction 2 hours, then by reactant
Centrifugal filtration, obtains the common 370g of filtrate, ammonium chloride 75g；(2) the filtrate (1) step isolated, will by flash column vacuum distillation
Solvent under reduced pressure in filtrate is distillated, and obtains ethanol 28g, surplus materials as admittedly sand coupling agent in kettle, and gross weight is 335g, ethanol
Reusable edible.
Claims (6)
1. a kind of preparation method of solid sand coupling agent, with the essence in 3- (2- aminoethyls)-aminopropyl alkoxy silane production process
Raw material based on kettle material is evaporated, described 3- (2- aminoethyls)-aminopropyl alkoxy silane is by initial feed ethylenediamine and chloropropyl
Silane reaction is obtained；It is characterized in that：Step is as follows：(1) by 3- (2- aminoethyls)-aminopropyl alkoxy silane production process
Rectifying still material input reactor in, add solvent and aminated compounds in reactor, control temperature of reaction kettle is 20～150
DEG C, stirring reaction 1～15 hour, then by reactant separation of solid and liquid, isolates filtrate and amine hydrochlorate sediment；(2) by step
(1) the filtrate decompression distillation isolated, the solvent in filtrate is distillated by distilling apparatus, surplus materials in reactor after distillation
As consolidate sand coupling agent；Above-mentioned solvent is C1～C5Straight or branched alkane alcohol, consumption for rectifying still material quality 5%～
30%；Above-mentioned aminated compounds is liquefied ammonia, the one kind in diethylenetriamine, consumption for rectifying still material quality 3%～30%；On
State in preparation process, if not containing ammonium chloride in the amine hydrochlorate sediment (1) isolated of step, in amine hydrochlorate sediment
Middle addition sodium alkoxide, stirring reaction obtain alcohol, free aminated compounds and sodium chloride, then by reactant separation of solid and liquid, separate
Go out the mixture and Sodium chloride deposit thing of alcohol and free aminated compounds, Sodium chloride deposit thing obtains chlorination after drying
It is converted to raw material input step after sodium solid, alcohol and the free purified separation of amine mixture again（1）In recycle.
2. the preparation method of a kind of solid sand coupling agent according to claim 1, it is characterised in that：Described 3- (2- ammonia second
Base)-aminopropyl alkoxy silane is：3- (2- aminoethyls)-aminopropyltriethoxy dimethoxysilane, 3- (2- aminoethyls)-ammonia third
Base trimethoxy silane, 3- (2- aminoethyls)-aminopropyltriethoxy diethoxy silane, 3- (2- aminoethyls) three ethoxy of-aminopropyl
One or more mixture in base silane.
3. the preparation method of a kind of solid sand coupling agent according to claim 1, it is characterised in that：Step (1) described in it is molten
Agent is methyl alcohol or ethanol.
4. the preparation method of a kind of solid sand coupling agent according to claim 1, it is characterised in that：Step (1) described in amine
Class compound is diethylenetriamine.
5. the preparation method of a kind of solid sand coupling agent according to claim 1, it is characterised in that：The amine that (1) step is isolated
Hydrochloride precipitates thing is ammonium chloride, the one kind in diethylenetriamine hydrochloride or two kinds.
6. the preparation method of a kind of solid sand coupling agent according to claim 1, it is characterised in that：The sodium alkoxide is preferably liquid
Body sodium methoxide or liquid ethanol sodium.
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| EP0702017B1 (en) * | 1994-09-14 | 2001-11-14 | Degussa AG | Process for the preparation of aminofunctional organosilanes with low chlorine contamination |
| CN1746176A (en) * | 2004-09-11 | 2006-03-15 | 张家港市国泰华荣化工新材料有限公司 | Preparation of 3-[N-(2-aminoethyl)aminoalkyoxyalkyl silane |
| DE102008002182A1 (en) * | 2008-06-03 | 2009-12-10 | Evonik Degussa Gmbh | Process for the preparation of alkylaminoalkylalkoxysilanes |
| CN102093404B (en) * | 2010-10-29 | 2013-11-13 | 华南理工大学 | Method for recovering and treating waste materials in aminosilane preparation |
| CN102558219B (en) * | 2011-12-16 | 2015-04-01 | 齐鲁工业大学 | Production process of tertiary amine silane |
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Address after: 215600 No.35 Nanhai Road, Jiangsu Yangzijiang International Chemical Industrial Park, Zhangjiagang, Suzhou, Jiangsu Province Patentee after: Zhangjiagang Guotai-Huarong New Chemical Materials Co.,Ltd. Address before: Zhangjiagang Guotai Huarong chemical new material Co., Ltd., No.9 Nanhai Road, Yangzijiang International Chemical Industrial Park, Zhangjiagang City, Suzhou City, Jiangsu Province, 215633 Patentee before: Zhangjiagang Guotai-Huarong New Chemical Materials Co.,Ltd. |
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