CN104087182A - Preparation method of light-colored rosin glyceride - Google Patents

Preparation method of light-colored rosin glyceride Download PDF

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Publication number
CN104087182A
CN104087182A CN201410368975.XA CN201410368975A CN104087182A CN 104087182 A CN104087182 A CN 104087182A CN 201410368975 A CN201410368975 A CN 201410368975A CN 104087182 A CN104087182 A CN 104087182A
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Prior art keywords
weight part
rosin
hours
preparation
light
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CN201410368975.XA
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Chinese (zh)
Inventor
黄桂彬
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Guangxi Zhongchang Resin Co Ltd
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Guangxi Zhongchang Resin Co Ltd
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Priority to CN201410368975.XA priority Critical patent/CN104087182A/en
Publication of CN104087182A publication Critical patent/CN104087182A/en
Pending legal-status Critical Current

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Abstract

The invention discloses a preparation method of light-colored rosin glyceride, belonging to the technical field of deep processing of rosin. The preparation method comprises the following steps: putting zeolite into a lead nitrate solution, soaking, then taking out, firstly baking until the water content is 20-30%, then roasting at 300-450 DEG C, and cooling to obtain a substance A for later use; putting rosin into a reaction kettle, controlling the air intake quantity of nitrogen, heating and melting, adding the substance A, rising temperature and then performing heat-preservation reaction 1; adding glycerin, zinc oxide, sodium thiosulfate and calcium hypophosphite, firstly performing heat-preservation reaction at 200-220 DEG C, then rising the temperature to 270-280 DEG C and performing heat-preservation reaction; and performing vacuum pumping to remove low-boiling-point substances, cooling, and discharging material to obtain the light-colored rosin glyceride. According to the preparation method disclosed by the invention, oxidation of rosin is furthest reduced so as to prepare the light-colored rosin glyceride with very light colors.

Description

The preparation method of pale rosin glyceryl ester
Technical field
The invention belongs to rosin deep process technology field, relate in particular to a kind of preparation method of pale rosin glyceryl ester.
Background technology
Rosin is taking pine resin as raw material, the non-volatile natural resin obtaining by different processing modes.Rosin is important industrial chemicals, is widely used in the industries such as soap, papermaking, paint, rubber.In addition, rosin also can be made ester gum by deep processing, and compared with rosin, its acid number significantly reduces, and embrittlement and being clamminess property reduce, and weathering resistance improves.But, due to rosin in deep-processing process with oxidation, cause the color of the ester gum making excessively dark, cannot reach the demand in market.
Summary of the invention
The technical problem that the present invention solves is to provide a kind of preparation method of pale rosin glyceryl ester, and the ester gum that the method makes is of light color.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:
A preparation method for pale rosin glyceryl ester, comprises the following steps:
A. zeolite is placed in to the lead nitrate solution that concentration is 0.1mol/L, soaks 1 day~2 days; Then take out, first at 80 DEG C~95 DEG C, dry to water content be 20%~30%, and then roasting 6 hours~8 hours at 300 DEG C~450 DEG C, the cooling substance A that obtains, for subsequent use;
B. 50 weight part~60 weight part rosin are put into reactor, nitrogen as protectant condition under, the air input of nitrogen is adjusted to 5ml/min~8ml/min, heating melts it completely, then the substance A that adds 1 weight part~2 weight part A step to make, stir and be warming up to 200 DEG C~220 DEG C, insulation reaction 1 hour~4 hours;
After C.B step, in described reactor, add 5 weight part~8 weight part glycerine, 0.5 weight part~0.8 part by weight of zinc oxide, 0.5 weight part~0.8 weight part Sulfothiorine and 0.4 weight part~0.6 weight part calcium propionate, stir, continue at 200 DEG C~220 DEG C insulation reaction 0.5 hour~1 hour; And then be warming up to 270 DEG C~280 DEG C, insulation reaction 2 hours~4 hours;
After D.C step, vacuumize and remove low-boiling-point substance, be then cooled to 200 DEG C~210 DEG C, discharging, obtains this pale rosin glyceryl ester.
Owing to adopting technique scheme, the beneficial effect that the present invention obtains is:
The present invention is by reducing as much as possible the oxidation of rosin, thereby makes the very shallow pale rosin glyceryl ester of color.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described, and protection scope of the present invention is not only confined to following examples.
Embodiment 1
The preparation method of this pale rosin glyceryl ester comprises the following steps:
A. zeolite is placed in to the lead nitrate solution that concentration is 0.1mol/L, soaks 1 day; Then take out, first at 80 DEG C, dry to water content be 20%, and then roasting 8 hours at 300 DEG C, the cooling substance A that obtains, for subsequent use;
B. 50kg rosin is put into reactor, nitrogen as protectant condition under, the air input of nitrogen is adjusted to 5ml/min, heating it is melted completely, the substance A that then adds 1kgA step to make, stirs and is warming up to 200 DEG C, insulation reaction 4 hours;
After C.B step, in described reactor, add 5kg glycerine, 0.5kg zinc oxide, 0.5kg Sulfothiorine and 0.4kg calcium propionate, stir, and continues at 200 DEG C insulation reaction 1 hour; And then be warming up to 270 DEG C, insulation reaction 4 hours;
After D.C step, vacuumize and remove low-boiling-point substance, be then cooled to 210 DEG C, discharging, obtains this pale rosin glyceryl ester.
Ghana's look of the pale rosin glyceryl ester that the present embodiment makes number is 4, and softening temperature is 110 DEG C.
Embodiment 2
The preparation method of this pale rosin glyceryl ester comprises the following steps:
A. zeolite is placed in to the lead nitrate solution that concentration is 0.1mol/L, soaks 2 days; Then take out, first at 95 DEG C, dry to water content be 30%, and then roasting 6 hours at 450 DEG C, the cooling substance A that obtains, for subsequent use;
B. 60kg rosin is put into reactor, nitrogen as protectant condition under, the air input of nitrogen is adjusted to 8ml/min, heating it is melted completely, the substance A that then adds 2kgA step to make, stirs and is warming up to 220 DEG C, insulation reaction 1 hour;
After C.B step, in described reactor, add 8kg glycerine, 0.8kg zinc oxide, 0.8kg Sulfothiorine and 0.6kg calcium propionate, stir, and continues at 220 DEG C insulation reaction 0.5 hour; And then be warming up to 280 DEG C, insulation reaction 2 hours;
After D.C step, vacuumize and remove low-boiling-point substance, be then cooled to 200 DEG C, discharging, obtains this pale rosin glyceryl ester.
Ghana's look of the pale rosin glyceryl ester that the present embodiment makes number is 4, and softening temperature is 108 DEG C.
Embodiment 3
The preparation method of this pale rosin glyceryl ester comprises the following steps:
A. zeolite is placed in to the lead nitrate solution that concentration is 0.1mol/L, soaks 1.5 days; Then take out, first at 90 DEG C, dry to water content be 25%, and then roasting 7 hours at 400 DEG C, the cooling substance A that obtains, for subsequent use;
B. 55kg rosin is put into reactor, nitrogen as protectant condition under, the air input of nitrogen is adjusted to 7ml/min, heating melts it completely, then the substance A that adds 1.5kgA step to make, stirs and is warming up to 210 DEG C, insulation reaction 3 hours;
After C.B step, in described reactor, add 6kg glycerine, 0.6kg zinc oxide, 0.6kg Sulfothiorine and 0.5kg calcium propionate, stir, and continues at 210 DEG C insulation reaction 0.5 hour; And then be warming up to 275 DEG C, insulation reaction 3 hours;
After D.C step, vacuumize and remove low-boiling-point substance, be then cooled to 205 DEG C, discharging, obtains this pale rosin glyceryl ester.
Ghana's look of the pale rosin glyceryl ester that the present embodiment makes number is 4, and softening temperature is 110 DEG C.

Claims (1)

1. a preparation method for pale rosin glyceryl ester, is characterized in that comprising the following steps:
A. zeolite is placed in to the lead nitrate solution that concentration is 0.1mol/L, soaks 1 day~2 days; Then take out, first at 80 DEG C~95 DEG C, dry to water content be 20%~30%, and then roasting 6 hours~8 hours at 300 DEG C~450 DEG C, the cooling substance A that obtains, for subsequent use;
B. 50 weight part~60 weight part rosin are put into reactor, nitrogen as protectant condition under, the air input of nitrogen is adjusted to 5ml/min~8ml/min, heating melts it completely, then the substance A that adds 1 weight part~2 weight part A step to make, stir and be warming up to 200 DEG C~220 DEG C, insulation reaction 1 hour~4 hours;
After C.B step, in described reactor, add 5 weight part~8 weight part glycerine, 0.5 weight part~0.8 part by weight of zinc oxide, 0.5 weight part~0.8 weight part Sulfothiorine and 0.4 weight part~0.6 weight part calcium propionate, stir, continue at 200 DEG C~220 DEG C insulation reaction 0.5 hour~1 hour; And then be warming up to 270 DEG C~280 DEG C, insulation reaction 2 hours~4 hours;
After D.C step, vacuumize and remove low-boiling-point substance, be then cooled to 200 DEG C~210 DEG C, discharging, obtains this pale rosin glyceryl ester.
CN201410368975.XA 2014-07-30 2014-07-30 Preparation method of light-colored rosin glyceride Pending CN104087182A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106085243A (en) * 2016-06-27 2016-11-09 梧州市嘉盈树胶有限公司 The preparation method of pale rosin glyceride

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1085929A (en) * 1993-10-21 1994-04-27 福建省龙岩地区林产工业公司 The manufacture method of glycerin abietate modified by maleic anhydride
CN102634281A (en) * 2012-03-30 2012-08-15 玉林师范学院 Color-lightening agent for preparing pale rosin and application thereof
CN103214971A (en) * 2013-04-28 2013-07-24 上思县松香厂 Preparation method of pale rosin ester

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1085929A (en) * 1993-10-21 1994-04-27 福建省龙岩地区林产工业公司 The manufacture method of glycerin abietate modified by maleic anhydride
CN102634281A (en) * 2012-03-30 2012-08-15 玉林师范学院 Color-lightening agent for preparing pale rosin and application thereof
CN103214971A (en) * 2013-04-28 2013-07-24 上思县松香厂 Preparation method of pale rosin ester

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106085243A (en) * 2016-06-27 2016-11-09 梧州市嘉盈树胶有限公司 The preparation method of pale rosin glyceride

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Application publication date: 20141008