CN106118486A - The production method of Sucrose Ester of Rosin Acid - Google Patents

The production method of Sucrose Ester of Rosin Acid Download PDF

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Publication number
CN106118486A
CN106118486A CN201610469877.4A CN201610469877A CN106118486A CN 106118486 A CN106118486 A CN 106118486A CN 201610469877 A CN201610469877 A CN 201610469877A CN 106118486 A CN106118486 A CN 106118486A
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CN
China
Prior art keywords
production method
rosin acid
sucrose ester
sucrose
colophonium
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201610469877.4A
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Chinese (zh)
Inventor
黄桂彬
蒋茵荣
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Guangxi Zhongchang Resin Co Ltd
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Guangxi Zhongchang Resin Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Application filed by Guangxi Zhongchang Resin Co Ltd filed Critical Guangxi Zhongchang Resin Co Ltd
Priority to CN201610469877.4A priority Critical patent/CN106118486A/en
Publication of CN106118486A publication Critical patent/CN106118486A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09FNATURAL RESINS; FRENCH POLISH; DRYING-OILS; DRIERS (SICCATIVES); TURPENTINE
    • C09F1/00Obtaining purification, or chemical modification of natural resins, e.g. oleo-resins
    • C09F1/04Chemical modification, e.g. esterification

Abstract

The invention discloses the production method of a kind of Sucrose Ester of Rosin Acid, its production method is: alcohols material, Colophonium and sucrose are sequentially added in cavitation machine, is subsequently adding molecular sieve, opens cavitation machine, esterification, is filtered to remove molecular sieve, impurity is distilled off.Colophonium and sucrose single step reaction are prepared Sucrose Ester of Rosin Acid by the present invention, and assist cavitation device, and reaction can complete within a short period of time, and product purity is higher, gained solvent recoverable.

Description

The production method of Sucrose Ester of Rosin Acid
Technical field
The present invention relates to Colophonium deep process technology field, the production method of a kind of Sucrose Ester of Rosin Acid.
Background technology
Colophonium is a kind of reproducible natural resin, is widely used in coating, adhesive, ink, papermaking, soap, metal The industries such as processing, synthetic rubber, building materials, food, macromolecule, fine chemical product.But due to the unstability of Colophonium itself, as easily Crystallization, easy oxidized variable color and softening point are low so that it is performance and application are subject to certain restrictions.Colophonium is esterified Modification is one of the most important mode.
Sucrose Ester of Rosin Acid is a kind of good surfactant of biodegradability, can be used as the emulsifying agent of food, divides Powder and viscosity modifier etc., being mainly by Colophonium and sucrose is that primary raw material is prepared from.But, current Sucrose Ester of Rosin Acid Preparation method typically experience for a long time backflow, the time used is longer, accordingly, it would be desirable to seek one quickly prepare rosin acid sugarcane The method of sugar ester.
Summary of the invention
It is an object of the invention to provide the production method of a kind of Sucrose Ester of Rosin Acid, this production method can solve Colophonium The problem that the acid sucrose ester production time is longer.
In order to solve the problems referred to above, the technical solution used in the present invention is:
The production method of this Sucrose Ester of Rosin Acid is: be sequentially added into alcohols material, Colophonium and sucrose in cavitation machine, and mixing is all Even, it is subsequently adding catalysts, opens cavitation machine, control reaction temperature to 130 DEG C~150 DEG C, react 1 hour~1.5 little Time, filter, collect filtrate, insulation distillation 1 hour~2 hours.
In technique scheme, more specifically technical scheme is it may also is that catalyst is molecular sieve catalyst.
Further, the preparation method of molecular sieve catalyst is: according to 1:1~5:0.3~1:10~the mass ratio of 20, will Sodium silicate, aluminium oxide and sodium hydroxide and water mixing, proceed in microwave oven, and arranging microwave frequency is 500 hertz~800 hertz, Microwave 30 minutes~60 minutes.
Further, the one during alcohols material is methanol, ethanol, glycerol and butanol.
Further, the mass ratio of alcohols material, Colophonium, sucrose and catalyst be 1:6~8:8~12:0.05~ 0.2。
Further, vapo(u)rizing temperature is 150 DEG C~180 DEG C.
Owing to have employed technique scheme, the present invention compared with prior art has the advantages that
1, Colophonium and sucrose single step reaction are prepared Sucrose Ester of Rosin Acid by the present invention, and assist cavitation device, produce in course of reaction Raw High Temperature High Pressure makes chemical bond rupture and produces free radical etc., thus promotes that reaction is carried out largely so that reaction Within a short period of time can complete.
2, feed stock conversion of the present invention is high, side reaction is few, product purity is higher.
3, the present invention distills gained solvent and can recycle.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1
The production method of the present embodiment Sucrose Ester of Rosin Acid is: be sequentially added into ethanol, Colophonium and sucrose in cavitation machine, and mixing is all Even, it is subsequently adding molecular sieve, opens cavitation machine, the operating pressure of regulation cavitation machine is 0.4 MPa, controls reaction temperature to 150 DEG C, to react 1.2 hours, filter, collect filtrate, regulation vapo(u)rizing temperature is 150 DEG C, insulation distillation 1.2 hours.
In the present embodiment, the mass ratio of ethanol, Colophonium, sucrose and catalyst is 1:6:12:0.05.
The preparation method of the present embodiment molecular sieve catalyst is: according to the mass ratio of 1:1:0.3:10, by sodium silicate, oxidation Aluminum and sodium hydroxide and water mix, and proceed in microwave oven, and arranging microwave frequency is 800 hertz, and microwave 50 minutes i.e. obtains this reality Execute example catalyst.
Embodiment 2
The production method of the present embodiment Sucrose Ester of Rosin Acid is: be sequentially added into butanol, Colophonium and sucrose in cavitation machine, and mixing is all Even, it is subsequently adding molecular sieve, opens cavitation machine, the operating pressure of regulation cavitation machine is 0.6 MPa, controls reaction temperature to 140 DEG C, to react 1 hour, filter, collect filtrate, regulation vapo(u)rizing temperature is 160 DEG C, insulation distillation 1 hour.
In the present embodiment, the mass ratio of butanol, Colophonium, sucrose and catalyst is 1:7:11:0.1.
The preparation method of the present embodiment molecular sieve catalyst is: according to the mass ratio of 1:2:0.5:15, by sodium silicate, oxidation Aluminum and sodium hydroxide and water mix, and proceed in microwave oven, and arranging microwave frequency is 600 hertz, and microwave 40 minutes i.e. obtains this reality Execute example catalyst.
Embodiment 3
The production method of the present embodiment Sucrose Ester of Rosin Acid is: be sequentially added into methanol, Colophonium and sucrose in cavitation machine, and mixing is all Even, it is subsequently adding molecular sieve, opens cavitation machine, the operating pressure of regulation cavitation machine is 0.7 MPa, controls reaction temperature to 135 DEG C, to react 1.1 hours, filter, collect filtrate, regulation vapo(u)rizing temperature is 170 DEG C, insulation distillation 1.6 hours.
In the present embodiment, the mass ratio of methanol, Colophonium, sucrose and catalyst is 1:8:10:0.15.
The preparation method of the present embodiment molecular sieve catalyst is: according to the mass ratio of 1:5:1:16, by sodium silicate, aluminium oxide Mixing with sodium hydroxide and water, proceed in microwave oven, arranging microwave frequency is 700 hertz, and microwave 60 minutes i.e. obtains this enforcement Example catalyst.
Embodiment 4
The production method of the present embodiment Sucrose Ester of Rosin Acid is: be sequentially added into glycerol, Colophonium and sucrose in cavitation machine, mixing Uniformly, being subsequently adding molecular sieve, open cavitation machine, the operating pressure of regulation cavitation machine is 0.8 MPa, controls reaction temperature extremely 130 DEG C, reacting 1.5 hours, filter, collect filtrate, regulation vapo(u)rizing temperature is 180 DEG C, insulation distillation 1 hour.
In the present embodiment, the mass ratio of glycerol, Colophonium, sucrose and catalyst is 1:8:8:0.2.
The preparation method of the present embodiment molecular sieve catalyst is: according to the mass ratio of 1:3:0.8:20, by sodium silicate, oxidation Aluminum and sodium hydroxide and water mix, and proceed in microwave oven, and arranging microwave frequency is 800 hertz, and microwave 30 minutes i.e. obtains this reality Execute example catalyst.

Claims (7)

1. the production method of Sucrose Ester of Rosin Acid, it is characterised in that comprise the following steps: be sequentially added into alcohols thing in cavitation machine Matter, Colophonium and sucrose, mix homogeneously, it is subsequently adding catalysts, opens cavitation machine, control reaction temperature to 130 DEG C~150 DEG C, react 1 hour~1.5 hours, filter, collect filtrate, insulation distillation 1 hour~2 hours.
The production method of Sucrose Ester of Rosin Acid the most according to claim 1, it is characterised in that: described catalyst is molecular sieve Catalyst.
The production method of Sucrose Ester of Rosin Acid the most according to claim 2, it is characterised in that described molecular sieve catalyst Preparation method is: according to 1:1~5:0.3~1:10~the mass ratio of 20, sodium silicate, aluminium oxide and sodium hydroxide and water are mixed Closing, proceed in microwave oven, arranging microwave frequency is 500 hertz~800 hertz, microwave 30 minutes~60 minutes.
4. according to the production method of the Sucrose Ester of Rosin Acid described in claim 1 or 2 or 3, it is characterised in that: described alcohols material For the one in methanol, ethanol, glycerol and butanol.
5. according to the production method of the Sucrose Ester of Rosin Acid described in claim 1 or 2 or 3, it is characterised in that: described alcohols thing The mass ratio of matter, Colophonium, sucrose and catalyst is 1:6~8:8~12:0.05~0.2.
6. according to the production method of the Sucrose Ester of Rosin Acid described in claim 1 or 2 or 3, it is characterised in that: described vapo(u)rizing temperature It it is 150 DEG C~180 DEG C.
7. according to the production method of the Sucrose Ester of Rosin Acid described in claim 1 or 2 or 3, it is characterised in that: described cavitation machine Operating pressure is 0.4 MPa~0.8 MPa.
CN201610469877.4A 2016-06-26 2016-06-26 The production method of Sucrose Ester of Rosin Acid Pending CN106118486A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110229197A (en) * 2019-07-06 2019-09-13 潍坊大耀新材料有限公司 A kind of preparation method of the one's own physical property sucrose ester of small molecule without solvent

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05156209A (en) * 1991-12-10 1993-06-22 Arakawa Chem Ind Co Ltd Production of rosin alcohol
JP2014070167A (en) * 2012-09-28 2014-04-21 Seiko Pmc Corp Rosin polyhydric alcohol ester resin, ink emulsification suitability improver, varnish for offset printing ink, and ink composition for offset printing
CN103952082A (en) * 2014-04-22 2014-07-30 南京林业大学 Method for preparing abietinol
CN203820747U (en) * 2014-04-17 2014-09-10 河南亚太能源科技有限公司 Efficient cavitation device
CN104031100A (en) * 2014-06-29 2014-09-10 陈昆 Method for preparing sucrose abietate

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH05156209A (en) * 1991-12-10 1993-06-22 Arakawa Chem Ind Co Ltd Production of rosin alcohol
JP2014070167A (en) * 2012-09-28 2014-04-21 Seiko Pmc Corp Rosin polyhydric alcohol ester resin, ink emulsification suitability improver, varnish for offset printing ink, and ink composition for offset printing
CN203820747U (en) * 2014-04-17 2014-09-10 河南亚太能源科技有限公司 Efficient cavitation device
CN103952082A (en) * 2014-04-22 2014-07-30 南京林业大学 Method for preparing abietinol
CN104031100A (en) * 2014-06-29 2014-09-10 陈昆 Method for preparing sucrose abietate

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
孟繁智: "《新编精细化工应用配方10000例与生产工艺实用手册 上》", 29 February 2004, 银声音像出版社 *
龙英才: "沸石分子筛催化材料──高科技的硅铝酸盐产品", 《2007全国无机硅化物行业年会论文集》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110229197A (en) * 2019-07-06 2019-09-13 潍坊大耀新材料有限公司 A kind of preparation method of the one's own physical property sucrose ester of small molecule without solvent

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