CN105754485B - The production method of rosin glycerides - Google Patents

The production method of rosin glycerides Download PDF

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Publication number
CN105754485B
CN105754485B CN201610233688.7A CN201610233688A CN105754485B CN 105754485 B CN105754485 B CN 105754485B CN 201610233688 A CN201610233688 A CN 201610233688A CN 105754485 B CN105754485 B CN 105754485B
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parts
rosin
glycerine
thiobis
anthraquinone
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CN105754485A (en
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叶旗
周卓瑜
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WUZHOU FEIZHUOLIN PRODUCT INDUSTRIAL Co Ltd
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WUZHOU FEIZHUOLIN PRODUCT INDUSTRIAL Co Ltd
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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; OIL DRYING AGENTS, i.e. SICCATIVES; TURPENTINE
    • C09F1/00Obtaining purification, or chemical modification of natural resins, e.g. oleo-resins
    • C09F1/04Chemical modification, e.g. esterification

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The present invention discloses a kind of production method of rosin glycerides, belongs to rosin deep process technology field.The present invention uses the raw material of following parts by weight:100 parts of rosin, 0.0001 part~0.0002 part of anthraquinone, 0.0001 part~0.0002 part of tetraethyl orthosilicate, 5 parts~8 parts of hydroquinone, 4,4` thiobis(6 tertiary butyl, 3 methylphenol)0.01 part~0.02 part of 0.001 part~0.002 part, 15 parts~25 parts of glycerine and sodium acetate;Wherein, including first rosin is refined, is then added tetraethyl orthosilicate, hydroquinone, glycerine and sodium acetate under agitation, and specified pressure, at a temperature of reacted;Then anthraquinone and 4,4` thiobis are just added again(6 tertiary butyl, 3 methylphenol), and specified pressure, at a temperature of distilled.The advantage that product rosin glycerides softening point produced by the present invention is high, purity is high.

Description

The production method of rosin glycerides
Technical field
The invention belongs to rosin deep process technology field more particularly to a kind of production methods of rosin glycerides.
Background technology
Rosin glycerides are a kind of irregular transparent cake, sheet or granular solids, have inoxidizability and thermal stability It is good, it is ageing-resistant, with high molecular material good compatibility(NR, CR, SBR, SIS, EVA etc.), initial bonding strength is good, can be used in yellow glue and change Kind initial bond, it is also possible to make thermosol pressure sensitive adhesive, the molten pressure sensitive adhesive of oil, adhesive sticker, Laminating adhesive, EVA hot-melt adhesive, polyamide hot melt The tackifying resin of glue, fluid sealant, varnish paint vehicle, bookbinding glue, pipeline glue, Laminating adhesive, decorating glue, trademark adhesive, adhesive tape glue etc..
The traditional preparation methods of rosin glycerides are synthesized after modified with glycerine esterification by rosin or pale rosin, are passed through Made of after distillation.The purity of rosin glycerides made from this method is generally relatively low so that the popularization and application of rosin glycerides by Limitation is arrived.
Invention content
Technical problem to be solved by the invention is to provide a kind of high softening-point, the producers of high-purity rosin glycerides Method.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is:
It uses the raw material of following parts by weight:
100 parts of rosin, 0.0001 part~0.0002 part of anthraquinone, 0.0001 part~0.0002 part of tetraethyl orthosilicate, to benzene 5 parts~8 parts of diphenol, 4,4`- thiobis(6- tertiary butyl -3- methylphenols)0.001 part~0.002 part, 15 parts~25 parts of glycerine And 0.01 part~0.02 part of sodium acetate;
Including following preparation process:
A, based on above-mentioned parts by weight, raw material rosin is vacuumized into vacuum distillation and obtains refined rosin;
B, under stirring, refined rosin made from step A is put into reaction kettle, and sequentially adds above-mentioned parts by weight Tetraethyl orthosilicate, hydroquinone, glycerine and sodium acetate be heated to 200 then under the pressure of 0MPa~0.01MPa DEG C~220 DEG C, constant temperature stirring, reaction 2 hours~4 hours;
C, substance made from step B is put into destilling tower, and is put into anthraquinone, 4,4`- thiobis(6- tertiary butyl -3- first Base phenol), then distilled under conditions of pressure is 0MPa~0.01MPa, temperature is 270 DEG C~280 DEG C, rosin be made Glyceride.
In above-mentioned technical proposal, more specific technical solution is:100 parts of rosin, 0.0001 part of anthraquinone, tetraethyl orthosilicate 0.0001 part, 5 parts of hydroquinone, 4,4`- thiobis(6- tertiary butyl -3- methylphenols)0.001 part, 15 parts of glycerine and acetic acid 0.02 part of sodium;
Further, 100 parts of rosin, 0.00016 part of anthraquinone, tetraethyl orthosilicate 0.00016,6 parts of hydroquinone, 4, 4`- thiobis(6- tertiary butyl -3- methylphenols)0.017 part of 0.0015 part, 25 parts of glycerine and sodium acetate;
Further, 100 parts of rosin, 0.0002 part of anthraquinone, 0.0002 part of tetraethyl orthosilicate, 8 parts of hydroquinone, 4, 4`- thiobis(6- tertiary butyl -3- methylphenols)0.01 part of 0.002 part, 20 parts of glycerine and sodium acetate.
Due to the adoption of the above technical scheme, the present invention has the advantages that:
The present invention by the way that first rosin is refined, then under agitation be added tetraethyl orthosilicate, hydroquinone, Glycerine and sodium acetate, and specified pressure, at a temperature of reacted;Then anthraquinone and 4,4`- thiobis are just added again(Uncle 6- Butyl -3- methylphenols), and specified pressure, at a temperature of distilled, it is sweet to which high softening-point, the rosin of high-purity be made Grease.
Specific implementation mode
Below in conjunction with specific example, the invention will be further described:
Embodiment 1
This rosin glycerides includes following preparation process:
A, raw material 100kg rosin is vacuumized into vacuum distillation and obtains refined rosin;
B, under stirring, refined rosin made from step A is put into reaction kettle, and sequentially adds positive silicic acid tetrem Ester 0.0001kg, hydroquinone 5kg, glycerine 15kg and sodium acetate 0.02kg are heated to 220 then under the pressure of 0MPa DEG C, constant temperature stirring, reaction 2 hours;
C, substance made from step B is put into destilling tower, and is put into anthraquinone 0.0001kg, 4,4`- thiobis(The tertiary fourths of 6- Base -3- methylphenols)Then 0.001kg is distilled under conditions of pressure is 0MPa, temperature is 280 DEG C, it is sweet that rosin is made Grease.
The softening point of rosin glycerides made from the present embodiment is up to 120 DEG C, and purity is up to 99%.
Embodiment 2
This rosin glycerides includes following preparation process:
A, raw material 100kg rosin is vacuumized into vacuum distillation and obtains refined rosin;
B, under stirring, refined rosin made from step A is put into reaction kettle, and sequentially adds positive silicic acid tetrem Ester 0.00016kg, hydroquinone 6kg, glycerine 25kg and sodium acetate 0.017kg, then under the pressure of 0.01MPa, heating To 200 DEG C, constant temperature stirring is reacted 4 hours;
C, substance made from step B is put into destilling tower, and is put into anthraquinone 0.00016kg, 4,4`- thiobis(Uncle 6- Butyl -3- methylphenols)Then 0.0015kg is distilled under conditions of pressure is 0.01MPa, temperature is 270 DEG C, be made Rosin glycerides.
The softening point of rosin glycerides made from the present embodiment is up to 125 DEG C, and purity is up to 99.1%.
Embodiment 3
This rosin glycerides includes following preparation process:
A, raw material 100kg rosin is vacuumized into vacuum distillation and obtains refined rosin;
B, under stirring, refined rosin made from step A is put into reaction kettle, and sequentially adds positive silicic acid tetrem Ester 0.0002kg, hydroquinone 8kg, glycerine 20kg and sodium acetate 0.01kg are heated to then under the pressure of 0.005MPa 205 DEG C, constant temperature stirring, reaction 3 hours;
C, substance made from step B is put into destilling tower, and is put into anthraquinone 0.0002kg, 4,4`- thiobis(The tertiary fourths of 6- Base -3- methylphenols)Then 0.002kg is distilled under conditions of pressure is 0.005MPa, temperature is 205 DEG C, pine is made Fragrant glyceride..
The softening point of rosin glycerides made from the present embodiment is up to 120 DEG C, and purity is up to 99.5%.

Claims (4)

1. a kind of production method of rosin glycerides, it is characterised in that:
Using the raw material of following parts by weight:
100 parts of rosin, 0.0001 part~0.0002 part of anthraquinone, 0.0001 part~0.0002 part of tetraethyl orthosilicate, hydroquinone 5 Part~8 parts, 4,4`- thiobis(6- tertiary butyl -3- methylphenols)0.001 part~0.002 part, 15 parts~25 parts of glycerine and vinegar 0.01 part~0.02 part of sour sodium;
Including following preparation process:
A, based on above-mentioned parts by weight, raw material rosin is vacuumized into vacuum distillation and obtains refined rosin;
B, under stirring, refined rosin made from step A is put into reaction kettle, and sequentially adds above-mentioned parts by weight just Tetraethyl orthosilicate, hydroquinone, glycerine and sodium acetate, then constant temperature is stirred, is reacted 2 hours under three phase point pressure below ~4 hours;
C, substance made from step B is put into destilling tower, and is put into anthraquinone, 4,4`- thiobis(6- tertiary butyl -3- methylbenzenes Phenol), then distilled under conditions of pressure is -0.1MPa~0MPa, temperature is 180 DEG C~200 DEG C, rosin glycerine be made Ester.
2. the production method of rosin glycerides according to claim 1, it is characterised in that:100 parts of rosin, anthraquinone 0.0001 Part, 0.0001 part of tetraethyl orthosilicate, 5 parts of hydroquinone, 4,4`- thiobis(6- tertiary butyl -3- methylphenols)0.001 part, 0.02 part of 15 parts of glycerine and sodium acetate.
3. the production method of rosin glycerides according to claim 1, it is characterised in that:100 parts of rosin, anthraquinone 0.00016 part, 0.00016 part of tetraethyl orthosilicate, 6 parts of hydroquinone, 4,4`- thiobis(6- tertiary butyl -3- methylphenols) 0.017 part of 0.0015 part, 25 parts of glycerine and sodium acetate.
4. the production method of rosin glycerides according to claim 1, it is characterised in that:100 parts of rosin, anthraquinone 0.0002 Part, 0.0002 part of tetraethyl orthosilicate, 8 parts of hydroquinone, 4,4`- thiobis(6- tertiary butyl -3- methylphenols)0.002 part, 0.01 part of 20 parts of glycerine and sodium acetate.
CN201610233688.7A 2016-04-15 2016-04-15 The production method of rosin glycerides Active CN105754485B (en)

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CN106299376B (en) * 2016-10-12 2019-01-04 漳州万宝能源科技有限公司 A kind of high capacity high safety performance lithium battery anode and preparation method thereof
EP3635056B1 (en) 2017-06-30 2024-04-10 Kraton Polymers LLC Light color rosin ester compositions and methods of making same

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102631940A (en) * 2012-03-30 2012-08-15 玉林师范学院 Composite catalyst and application thereof in preparing pale rosin glyceride
CN103045097A (en) * 2012-12-06 2013-04-17 何丽萍 Preparation method of rosin glycerol ester
CN103436176A (en) * 2013-08-28 2013-12-11 梧州市嘉盈树胶有限公司 Preparation method of high-softening-point rosin glycerin ester
CN103436174A (en) * 2013-08-27 2013-12-11 广西梧州松脂股份有限公司 Preparation method of rosin glycerin ester
CN104694015A (en) * 2015-03-18 2015-06-10 桂林兴松林化有限责任公司 Preparation method of light-color glycerol ester of rosin
CN104774560A (en) * 2014-01-09 2015-07-15 江西麻山化工有限公司 Preparation method of rosin glycerin ester

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102631940A (en) * 2012-03-30 2012-08-15 玉林师范学院 Composite catalyst and application thereof in preparing pale rosin glyceride
CN103045097A (en) * 2012-12-06 2013-04-17 何丽萍 Preparation method of rosin glycerol ester
CN103436174A (en) * 2013-08-27 2013-12-11 广西梧州松脂股份有限公司 Preparation method of rosin glycerin ester
CN103436176A (en) * 2013-08-28 2013-12-11 梧州市嘉盈树胶有限公司 Preparation method of high-softening-point rosin glycerin ester
CN104774560A (en) * 2014-01-09 2015-07-15 江西麻山化工有限公司 Preparation method of rosin glycerin ester
CN104694015A (en) * 2015-03-18 2015-06-10 桂林兴松林化有限责任公司 Preparation method of light-color glycerol ester of rosin

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Application publication date: 20160713

Assignee: GUANGXI ZHONGCHANG RESIN Co.,Ltd.

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