CN106831663A - A kind of allyl glycidyl ether dewatering - Google Patents
A kind of allyl glycidyl ether dewatering Download PDFInfo
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- CN106831663A CN106831663A CN201710115476.3A CN201710115476A CN106831663A CN 106831663 A CN106831663 A CN 106831663A CN 201710115476 A CN201710115476 A CN 201710115476A CN 106831663 A CN106831663 A CN 106831663A
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- Prior art keywords
- allyl glycidyl
- glycidyl ether
- molecular sieves
- warming
- dewatering
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D303/00—Compounds containing three-membered rings having one oxygen atom as the only ring hetero atom
- C07D303/02—Compounds containing oxirane rings
- C07D303/12—Compounds containing oxirane rings with hydrocarbon radicals, substituted by singly or doubly bound oxygen atoms
- C07D303/18—Compounds containing oxirane rings with hydrocarbon radicals, substituted by singly or doubly bound oxygen atoms by etherified hydroxyl radicals
- C07D303/20—Ethers with hydroxy compounds containing no oxirane rings
- C07D303/22—Ethers with hydroxy compounds containing no oxirane rings with monohydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/14—Type A
- C01B39/16—Type A from aqueous solutions of an alkali metal aluminate and an alkali metal silicate excluding any other source of alumina or silica but seeds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D301/00—Preparation of oxiranes
- C07D301/32—Separation; Purification
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- General Life Sciences & Earth Sciences (AREA)
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Abstract
The invention discloses a kind of allyl glycidyl ether dewatering, it is related to organic object depth degree dehydration field, the method is comprised the following steps：3A molecular sieves are prepared, 3A analysis sieves is inserted in atmospheric distillation tower as filler, first infinite reflux 2~4 hours, be then 3~5 collection products by reflux ratio, intercept tails.Wherein, the step of preparation 3A molecular sieves are：In molar ratio, after 1~1.2 part of waterglass, 1 part of sodium metaaluminate and 1~1.2 NaOH being well mixed, 70 DEG C~80 DEG C is warming up to and 30~50 minutes generation gels are incubated, then be warming up to 90~110 DEG C of 3~6h of crystallization, obtain crystal powder；Ion exchange is carried out to 1~1.2 part of potassium chloride is added in 1 part of crystal powder, obtain potassium metaaluminate solution, by the filtering of potassium metaaluminate solution, washing, drying, add adhesive, calcination 4~10 hours, obtain 3A analysis sieves, the present invention can the relatively low allyl glycidyl ether of isolated water content, and impurity will not be introduced.
Description
Technical field
The present invention relates to organic matter deep dehydration field, and in particular to a kind of allyl glycidyl ether dewatering.
Background technology
γ-glycidyl ether oxygen propyl trimethoxy silicane (KH-560) is a kind of extremely wide silane coupler of purposes, by
Epoxide group reactivity in KH-560 molecules is relatively strong, easily crosslinks reaction with other compounds, therefore, KH-560 is usual
In as additive addition composite, to improve the mechanical strength and electrical insulating property of composite, it is widely used in plastics, applies
The fields such as material, adhesive.
The commercial synthesis raw material of KH-560 is allyl glycidyl ether and trimethyl hydrogen silane, because allyl glycidyl is sweet
The water content of oily ether is higher, and more high-boiling components are easily generated in course of reaction, has had a strong impact on the yield of product, while high-boiling components
Generation also have serious influence to the water solubility of product, be unfavorable for that its normal in the various fields in downstream being used.
In order to reduce the water content of allyl glycidyl ether, azeotropic-extraction generally is used to allyl glycidyl ether
The methods such as rectification method, extractive distillation with salt carry out rectifying water removal, high-purity of the water content less than 1000ppm is can obtain after rectifying and is produced
Product.But, azeotropic-extraction fractional distillation, extractive distillation with salt technique it is more complicated, energy consumption is higher, and can introduce the third material,
Cause the novel substance still needed to after separating further to introducing to separate, cause complex process, yield reduction.
The content of the invention
For defect present in prior art, it is an object of the invention to provide a kind of dehydration of allyl glycidyl ether
Method, can the relatively low allyl glycidyl ether of isolated water content, and impurity will not be introduced.
To achieve the above objectives, the present invention is adopted the technical scheme that：
A kind of allyl glycidyl ether dewatering, comprises the following steps：Prepare 3A molecular sieves, using 3A analysis sieve as
Filler is inserted in atmospheric distillation tower, first infinite reflux 2~4 hours, is then 3~5 collection products by reflux ratio, intercepts tails.
On the basis of above-mentioned technical proposal, the reflux ratio is 4.
On the basis of above-mentioned technical proposal, the tails is allyl glycidyl ether, and allyl glycidol
The water content of ether is less than 150ppm.
On the basis of above-mentioned technical proposal, the water content of the allyl glycidyl ether is 120ppm.
On the basis of above-mentioned technical proposal, the water content of the allyl glycidyl ether is 100ppm.
A kind of preparation method of 3A molecular sieves for allyl glycidyl ether dehydration, comprises the following steps：
A, in molar ratio, by 1~1.2 part of waterglass, 1 part of sodium metaaluminate and 1~1.2 NaOH it is well mixed after, rise
Temperature is to 70 DEG C~80 DEG C and is incubated 30~50 minutes generation gels, then is warming up to 90~110 DEG C of 3~6h of crystallization, obtains crystal powder
End；
B, to adding 1~1.2 part of potassium chloride to carry out ion exchange in 1 part of crystal powder, obtain potassium metaaluminate solution, will be inclined
The filtering of aluminic acid potassium solution, washing, drying, add adhesive, and calcination 4~10 hours obtains 3A analysis sieves.
On the basis of above-mentioned technical proposal, the step A is comprised the following steps：In molar ratio, by 1~1.2 part of water glass
After glass, 1 part of sodium metaaluminate and 1~1.2 NaOH are well mixed, it is warming up to 75 DEG C and is incubated 30~50 minutes generation gels,
100 DEG C of crystallization 5h are warming up to again, obtain crystal powder.
On the basis of above-mentioned technical proposal, the specific surface area of the 3A molecular sieves is 750~900m2/g。
Compared with prior art, the advantage of the invention is that：
(1) present invention in a kind of allyl glycidyl ether dewatering, by prepare heat endurance it is high, with uniform
Microcellular structure, specific surface area be 750~900m2The 3A molecular sieves of/g, and 3A molecular sieves are inserted in rectifying column as filler,
Add allyl glycidyl ether to be dehydrated, because the theoretical diameter of hydrone is 2.6A, allyl glycidyl ether point
Son is with diameter greater than 3A, therefore 3A molecular sieves can carry out deep dehydration to aqueous allyl glycidyl ether, can be contained
Allyl glycidyl ether of the water in below 150ppm.
Meanwhile, the present invention carries out deep dehydration in the way of physical absorption, obviates traditional rectifying and dewatering method (azeotropic essence
Evaporate method, extraction fractional distillation, extractive distillation with salt method) complex process, high energy consumption introduces the third material in system, cause to separate
After still need to the shortcomings of further being separated to the material, not only technics comparing is simple for the present invention, and is not required to introduce other materials, it is to avoid
Introduce impurity, it is possible to increase yield.
Specific embodiment
The present invention is described in further detail with reference to embodiments.
The embodiment of the present invention provides a kind of allyl glycidyl ether dewatering, comprises the following steps：
3A molecular sieves are prepared, 3A analysis sieves is inserted in atmospheric distillation tower as filler, first infinite reflux 2~4 hours, then
It is 3~5 collection products by reflux ratio, intercepts tails, allyl glycidol of the water content in below 150ppm can be obtained
Ether.
Wherein, 3A molecular sieves are prepared to comprise the following steps：
A, in molar ratio, by 1~1.2 part of waterglass, 1 part of sodium metaaluminate and 1~1.2 NaOH it is well mixed after, rise
Temperature to 70 DEG C~80 DEG C (optimal is 75 DEG C) and be incubated 30~50 minutes generation gel, then be warming up to 90~110 DEG C it is (optimal to be
100 DEG C) 3~6h of crystallization (optimal is 5h), obtain crystal powder.
B, to adding 1~1.2 part of potassium chloride to carry out ion exchange in 1 part of crystal powder, obtain potassium metaaluminate solution, will be inclined
The filtering of aluminic acid potassium solution, washing, drying, add adhesive, and calcination 4~10 hours obtains 3A analysis sieves.
The 3A molecular sieve heat endurances prepared in the present embodiment are high, and with uniform microcellular structure, specific surface area is 750~
900m2/ g, can regenerate and recycle.
Below, by 5 embodiments, the present invention is described in detail.
Embodiment 1
It is in molar ratio 1 by waterglass, sodium metaaluminate, NaOH:1：Heated after 1.2 mixing, at a temperature of 75 DEG C
45 minutes generation gels of insulation, are continuously heating to 100 DEG C, crystallize 5 hours, obtain crystal powder.Through filtering, washing, to 1 part of crystalline substance
Add 1 part of potassium chloride ions to exchange in body powder, through filtering, washing, drying, add adhesive, calcination 4 hours obtains 3A
Analysis sieve.
The specific surface area that the 3A analyses for using the method for the present embodiment to prepare are sieved is 750m2/g。
Embodiment 2
The present embodiment is in addition to burn event is 6h, and other conditions are same as Example 1, the ratio of the 3A analysis sieves for obtaining
Surface area is 800m2/g。
Embodiment 3
It is in molar ratio 1 by waterglass, sodium metaaluminate, NaOH:1.2:Heated after 1 mixing, at a temperature of 70 DEG C
30 minutes generation gels of insulation, are continuously heating to 90 DEG C, crystallize 3 hours, obtain crystal powder.Through filtering, washing, to 1 part of crystalline substance
Add 1.1 parts of potassium chloride ions to exchange in body powder, through filtering, washing, drying, add adhesive, calcination 4 hours is obtained
3A analysis sieves.
The specific surface area that the 3A analyses for using the method for the present embodiment to prepare are sieved is 900m2/g。
It is filler, atmospheric distillation, first infinite reflux 2 hours, then by one to use the 3A molecular sieves obtained by case study on implementation
Fixed reflux ratio collection product, intercepts tails, can obtain allyl glycidyl ether of the water content in below 150ppm.
Embodiment 4
It is in molar ratio 1 by waterglass, sodium metaaluminate, NaOH:1:Heated after 1 mixing, protected at a temperature of 80 DEG C
45 minutes generation gels of temperature, are continuously heating to 110 DEG C, crystallize 5 hours, obtain crystal powder.Through filtering, washing, to 1 part of crystal
Add 1.2 parts of potassium chloride ions to exchange in powder, through filtering, washing, drying, add adhesive, calcination 4 hours obtains 3A
Analysis sieve.
The specific surface area that the 3A analyses for using the method for the present embodiment to prepare are sieved is 850m2/g。
Embodiment 5
In the present embodiment, except calcination time is 8h, other conditions are same as Example 1, the method system of the present embodiment
The specific surface area of the standby 3A analysis sieves for obtaining is 900m2/g。
Drawn by embodiment 1 to 5, when waterglass, sodium metaaluminate, NaOH in molar ratio 1:1：1.2, calcination 8 is small
When the 3A molecular sieves that prepare to analyze size under Electronic Speculum the most suitable, with 3A molecular sieves obtained in embodiment 5 as filler, infinite reflux
The allyl glycidyl ether water content 143ppm for obtaining for 2 hours, the allyl glycidyl ether water that infinite reflux is obtained for 3 hours contains
Amount 135ppm, it is contemplated that economic benefit, infinite reflux can obtain satisfactory allyl glycidyl ether in 2 hours.
The present invention is not limited to the above-described embodiments, for those skilled in the art, is not departing from
On the premise of the principle of the invention, some improvements and modifications can also be made, these improvements and modifications are also considered as protection of the invention
Within the scope of.The content not being described in detail in this specification belongs to prior art known to professional and technical personnel in the field.
Claims (8)
1. a kind of allyl glycidyl ether dewatering, it is characterised in that：Comprise the following steps：3A molecular sieves are prepared, by 3A
Analysis sieve is inserted in atmospheric distillation tower as filler, first infinite reflux 2~4 hours, is then 3~5 collection products by reflux ratio, is cut
Take tails.
2. a kind of allyl glycidyl ether dewatering as claimed in claim 1, it is characterised in that：The reflux ratio is 4.
3. a kind of allyl glycidyl ether dewatering as claimed in claim 1, it is characterised in that：The tails is alkene
Propyl glycidyl ether, and the water content of allyl glycidyl ether is less than 150ppm.
4. a kind of allyl glycidyl ether dewatering as claimed in claim 3, it is characterised in that：The allyl glycidyl
The water content of glycerin ether is 120ppm.
5. a kind of allyl glycidyl ether dewatering as claimed in claim 3, it is characterised in that：The allyl glycidyl
The water content of glycerin ether is 100ppm.
6. it is a kind of for any one of claim 1 to 5 allyl glycidyl ether dehydration 3A molecular sieves preparation side
Method, it is characterised in that comprise the following steps：
A, in molar ratio, by 1~1.2 part of waterglass, 1 part of sodium metaaluminate and 1~1.2 NaOH it is well mixed after, be warming up to
70 DEG C~80 DEG C and 30~50 minutes generation gels of insulation, then 90~110 DEG C of 3~6h of crystallization are warming up to, obtain crystal powder；
B, in 1 part of crystal powder add 1~1.2 part of potassium chloride carry out ion exchange, potassium metaaluminate solution is obtained, by meta-aluminic acid
Potassium solution filtering, washing, drying, add adhesive, and calcination 4~10 hours obtains 3A analysis sieves.
7. a kind of preparation method of 3A molecular sieves as claimed in claim 6, it is characterised in that：The step A includes following step
Suddenly：In molar ratio, after 1~1.2 part of waterglass, 1 part of sodium metaaluminate and 1~1.2 NaOH being well mixed, 75 DEG C are warming up to
And 30~50 minutes generation gels are incubated, then 100 DEG C of crystallization 5h are warming up to, obtain crystal powder.
8. a kind of preparation method of 3A molecular sieves as claimed in claim 6, it is characterised in that：The specific surface of the 3A molecular sieves
Product is 750~900m2/g。
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| CN201710115476.3A CN106831663A (en) | 2017-03-01 | 2017-03-01 | A kind of allyl glycidyl ether dewatering |
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| CN201710115476.3A CN106831663A (en) | 2017-03-01 | 2017-03-01 | A kind of allyl glycidyl ether dewatering |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104402855A (en) * | 2014-10-31 | 2015-03-11 | 中国海洋石油总公司 | Vinylene carbonate dehydration distillation technology |
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2017
- 2017-03-01 CN CN201710115476.3A patent/CN106831663A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104402855A (en) * | 2014-10-31 | 2015-03-11 | 中国海洋石油总公司 | Vinylene carbonate dehydration distillation technology |
Non-Patent Citations (3)
| Title |
|---|
| 大连红光化工厂: "A型分子筛的生产工艺介绍", 《辽宁化工》 * |
| 李谦定 等: "《基础化学实验》", 30 September 2013 * |
| 蒋中逖 等: "《湖南省化工产品手册》", 31 October 1988 * |
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Application publication date: 20170613 |