CN111825846B - Light-colored high-stability water-soluble rosin resin and preparation method thereof - Google Patents
Light-colored high-stability water-soluble rosin resin and preparation method thereof Download PDFInfo
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- CN111825846B CN111825846B CN202010808305.0A CN202010808305A CN111825846B CN 111825846 B CN111825846 B CN 111825846B CN 202010808305 A CN202010808305 A CN 202010808305A CN 111825846 B CN111825846 B CN 111825846B
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- C09F1/04—Chemical modification, e.g. esterification
Abstract
The invention discloses a preparation method of light-color high-stability water-soluble rosin resin, which comprises the following steps: (1) crushing rosin; (2) adding ethanol into the rosin crushed material, heating while stirring to completely dissolve rosin to prepare a rosin mixed solution; (3) adding activated clay, molybdenum and sunflower seed oil into the rosin mixed solution, then introducing hydrogen, and heating for addition reaction to obtain a rosin mixture; (4) adding 2, 2-dimethyl-1, 3-propylene glycol into the rosin mixture, adding vanadium pentoxide and diatomite, and performing esterification reaction to obtain a rosin resin semi-finished product; (5) and adding fatty alcohol-polyoxyethylene ether sodium sulfate into the rosin resin semi-finished product, preserving heat, discharging and cooling to prepare the light-colored high-stability water-soluble rosin resin. The rosin resin produced by the method has the advantages of light color, high thermal stability and the like, is low in production energy consumption, is easy to realize industrialization, and has good economic efficiency, ecological benefit and social efficiency.
Description
[ technical field ] A method for producing a semiconductor device
The invention belongs to the technical field of deep processing of rosin resin, and particularly relates to light-colored high-stability water-soluble rosin resin and a preparation method thereof.
[ background of the invention ]
Rosin, as a renewable natural resin, is known as "petroleum grown on trees". The rosin industry is one of four major branch industries in forestry in China, and the trade volume of rosin accounts for 60 percent of the total world amount. Rosin is widely applied to the fields of coatings, printing ink, paint, adhesives, welding aids, rubber, papermaking, food additives, biological products and the like, but the performance and the application field of the rosin are limited because the rosin has instability such as easy crystallization, easy oxidation and color change, low softening point and the like.
The water-soluble rosin resin is polyol rosin with light color, is prepared by using refined rosin as basic raw material and through the processes of hydrogenation, esterification, water-soluble treatment and the like, and is a novel low-pollution, energy-saving and resource-saving coating. The water-soluble treatment is to introduce hydrophilic groups or solubilizing groups into the resin to make it a coating material using water as a dissolving medium. However, the water-soluble rosin resin prepared by the prior art has the defects of poor chemical resistance, low hardness, poor weather resistance, high color and luster and the like, contains a large amount of solvents, can generate a large amount of volatile organic matters, can seriously harm the environment and the body health of personnel in the production and construction processes, and also has the problems of poor viscosity, opacity, high production difficulty, poor compatibility and the like.
Chinese patent application document "a production method of water-soluble rosin resin (application publication No. CN 106752966A)" discloses a production method of water-soluble rosin resin, which comprises adding 100 parts by weight of rosin and 20-40 parts by weight of ethanol into a reactor, and dissolving the rosin at 180 ℃ at 170-; then adding a composite catalyst consisting of lanthanum chloride and a molecular sieve, introducing hydrogen, reacting for 60-90min at 80-100 ℃, and filtering to remove the catalyst to obtain hydrogenated rosin; adding hydrogenated rosin and polyalcohol into an esterification reactor, adding an acid catalyst, and carrying out esterification reaction at the temperature of 230-270 ℃ for 2-3h to obtain rosin resin; finally, 10-20 parts of organic matter containing hydrophilic groups is added, the temperature is kept at 120-140 ℃ for 30-60min, the mixture is cooled to room temperature, and the water-soluble rosin resin is obtained after discharging. The rosin resin produced by the method has the advantages of good water solubility, high viscosity, high hardness, environmental friendliness, no odor, transparency and the like, but has the problems of high coloring and poor stability and cannot meet the requirements of popularization and application.
[ summary of the invention ]
The invention provides a light-colored high-stability water-soluble rosin resin and a preparation method thereof, and aims to solve the problems of high color and poor stability and the like of the existing water-soluble rosin resin.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of a light-color high-stability water-soluble rosin resin comprises the following steps:
(1) pulverizing rosin to obtain pulverized rosin;
(2) adding 250 parts of 130-250 parts of ethanol into 78-92 parts of the rosin crushed material prepared in the step (1) by weight, and heating under stirring to completely dissolve the rosin to prepare a rosin mixed solution;
(3) adding 2.4-3.6 parts by weight of activated clay, molybdenum and sunflower seed oil into the rosin mixed solution prepared in the step (2) by weight, introducing hydrogen, heating to perform addition reaction for 75-95min, and filtering to remove the activated clay and the molybdenum to prepare a rosin mixture;
(4) taking parts by weight as a unit, adding 25-42 parts of 2, 2-dimethyl-1, 3-propylene glycol into the rosin mixture prepared in the step (3), adding 2.8-4.2 parts of vanadium pentoxide and diatomite by total weight, carrying out esterification reaction at the temperature of 270-275 ℃ for 1.2-1.4h, and filtering to remove the vanadium pentoxide and the diatomite to prepare a rosin resin semi-finished product;
(5) and (3) after cooling, adding 8-15 parts by weight of fatty alcohol-polyoxyethylene ether sodium sulfate into the rosin resin semi-finished product prepared in the step (4), preserving the heat for 40-55min, discharging and cooling to prepare the light-colored high-stability water-soluble rosin resin.
Further, the mass concentration of the ethanol in the step (2) is 85-92%.
Further, the stirring speed in the step (2) is 100-200 r/min.
Further, the temperature in step (2) is raised to 162-167 ℃.
And (3) further, the weight ratio of the activated clay to the molybdenum to the sunflower seed oil in the step (3) is 7-16:30-85: 9-20.
And (3) further, the hydrogen pressure in the step (3) is 10-20 MPa.
Further, the temperature in step (3) is raised to 110-120 ℃ for the addition reaction.
And (5) further, the weight ratio of the vanadium pentoxide to the diatomite in the step (4) is 4-9: 1.2-2.3.
Further, the temperature of the heat preservation in the step (5) is 104-.
The invention has the following beneficial effects:
(1) compared with the water-soluble rosin resin prepared by the prior art, the water-soluble rosin resin prepared by the invention has obviously lighter and higher color and water solubility, at least 10 Hassen color numbers are lighter and at least 23 times higher; meanwhile, the water-soluble rosin resin prepared by the method and the prior art is heated at 180 ℃ for 8 hours, and then detection shows that the color of the water-soluble rosin resin prepared by the method is improved by 5-7 hasen color numbers, while the color of the water-soluble rosin resin prepared by the prior art is improved by 13-21 hasen color numbers, which shows that the water-soluble rosin resin prepared by the method has higher stability than the water-soluble rosin resin prepared by the prior art.
(2) In the preparation process, the activated clay, the molybdenum and the sunflower seed oil play a synergistic role in addition reaction, the color of the water-soluble rosin resin is obviously reduced, the molybdenum plays a role in catalytic hydrogenation, the activated clay can enable the molybdenum to adsorb and disperse, the intensity of the molybdenum catalytic hydrogenation is increased, and the sunflower seed oil can play a role in lightening the color of the resin, so that the color of the water-soluble rosin resin is obviously reduced under the synergistic effect of the activated clay, the molybdenum and the sunflower seed oil in the addition reaction.
(3) The rosin resin produced by the invention can use water as a dissolving medium, contains lower Volatile Organic Compounds (VOC), can reduce the harm to the environment and the physical health of personnel, and overcomes the defects of the oily rosin resin.
(4) The rosin resin produced by the invention has the advantages of high viscosity, high hardness, good water resistance, environmental protection, no odor, transparency and the like.
(5) The method has the advantages of simple operation, environmental protection, safety, low energy consumption, low production cost, easy realization of industrial production and the like, and has good economic efficiency, ecological benefit and social efficiency.
[ description of the drawings ]
FIG. 1 is a flow chart of the preparation process of the light-colored high-stability water-soluble rosin resin.
[ detailed description ] embodiments
In order to facilitate a better understanding of the invention, the following examples are given to illustrate, but not to limit the scope of the invention.
In the embodiment, as shown in fig. 1, the preparation method of the light-colored high-stability water-soluble rosin resin comprises the following steps:
(1) pulverizing rosin to obtain pulverized rosin;
(2) adding 130-250 parts of 85-92% ethanol by mass concentration into 78-92 parts of the rosin crushed material prepared in the step (1) by weight, and heating to 162-167 ℃ at the rotation speed of 100-200r/min to completely dissolve the rosin to prepare a rosin mixed solution;
(3) adding 2.4-3.6 parts by weight of activated clay, molybdenum and sunflower seed oil into the rosin mixed solution prepared in the step (2) by taking the parts by weight as a unit, wherein the weight ratio of the activated clay to the molybdenum to the sunflower seed oil is 7-16:30-85:9-20, then introducing hydrogen, the pressure of the hydrogen is 10-20MPa, heating to 110-120 ℃, carrying out addition reaction for 75-95min, and filtering to remove the activated clay and the molybdenum to prepare a rosin mixture;
(4) adding 25-42 parts by weight of 2, 2-dimethyl-1, 3-propylene glycol into the rosin mixture prepared in the step (3), adding 2.8-4.2 parts by weight of vanadium pentoxide and diatomite at a weight ratio of 4-9:1.2-2.3, carrying out esterification reaction at the temperature of 270-275 ℃ for 1.2-1.4h, and filtering to remove the vanadium pentoxide and the diatomite to prepare a rosin resin semi-finished product;
(5) and (3) after cooling, adding 8-15 parts by weight of fatty alcohol-polyoxyethylene ether sodium sulfate into the rosin resin semi-finished product prepared in the step (4), preserving the heat for 40-55min at the temperature of 104-117 ℃, discharging and cooling to prepare the light-colored high-stability water-soluble rosin resin.
The present invention is illustrated by the following more specific examples.
Example 1
As shown in figure 1, the preparation method of the light-colored high-stability water-soluble rosin resin comprises the following steps:
(1) pulverizing rosin to obtain pulverized rosin;
(2) taking parts by weight as a unit, adding 136 parts of 88 mass percent ethanol into 80 parts of the rosin crushed material prepared in the step (1), heating to 162 ℃ at the rotating speed of 100r/min, and completely dissolving rosin to prepare a rosin mixed solution;
(3) adding 2.5 parts by weight of activated clay, molybdenum and sunflower seed oil into the rosin mixed solution prepared in the step (2) by taking the parts by weight as a unit, wherein the weight ratio of the activated clay to the molybdenum to the sunflower seed oil is 8:33:10, then introducing hydrogen, the pressure of the hydrogen is 12MPa, heating to 113 ℃, carrying out addition reaction for 92min, and filtering to remove the activated clay and the molybdenum to prepare a rosin mixture;
(4) adding 25 parts by weight of 2, 2-dimethyl-1, 3-propylene glycol into the rosin mixture prepared in the step (3), adding 3 parts by weight of vanadium pentoxide and diatomite according to the weight ratio of 5:1.4, carrying out esterification reaction at the temperature of 270 ℃ for 1.4h, and filtering to remove the vanadium pentoxide and the diatomite to prepare a rosin resin semi-finished product;
(5) and (3) after cooling, adding 8 parts by weight of fatty alcohol-polyoxyethylene ether sodium sulfate into the rosin resin semi-finished product prepared in the step (4), keeping the temperature at 107 ℃ for 53min, discharging and cooling to prepare the light-colored high-stability water-soluble rosin resin.
Example 2
As shown in figure 1, the preparation method of the light-colored high-stability water-soluble rosin resin comprises the following steps:
(1) pulverizing rosin to obtain pulverized rosin;
(2) adding 200 parts by weight of 90% ethanol into 85 parts by weight of the rosin crushed material prepared in the step (1), heating to 165 ℃ at a rotation speed of 200r/min, and completely dissolving rosin to prepare a rosin mixed solution;
(3) adding 3 parts by weight of activated clay, molybdenum and sunflower seed oil into the rosin mixed solution prepared in the step (2) by taking the parts by weight as a unit, wherein the weight ratio of the activated clay to the molybdenum to the sunflower seed oil is 12:62:15, then introducing hydrogen, the pressure of the hydrogen is 20MPa, heating to 118 ℃, carrying out addition reaction for 78min, and filtering to remove the activated clay and the molybdenum to prepare a rosin mixture;
(4) adding 36 parts by weight of 2, 2-dimethyl-1, 3-propylene glycol into the rosin mixture prepared in the step (3), adding 3.7 parts by weight of vanadium pentoxide and diatomite in a weight ratio of 8:1.5, carrying out esterification reaction at the temperature of 273 ℃ for 1.3h, and filtering to remove the vanadium pentoxide and the diatomite to prepare a rosin resin semi-finished product;
(5) and (3) after cooling, adding 12 parts by weight of fatty alcohol-polyoxyethylene ether sodium sulfate into the rosin resin semi-finished product prepared in the step (4), keeping the temperature at 115 ℃ for 46min, discharging and cooling to prepare the light-color high-stability water-soluble rosin resin.
Example 3
As shown in figure 1, the preparation method of the light-colored high-stability water-soluble rosin resin comprises the following steps:
(1) pulverizing rosin to obtain pulverized rosin;
(2) adding 245 parts by weight of 89% ethanol into 90 parts by weight of the rosin crushed material prepared in the step (1), heating to 166 ℃ at the rotating speed of 100r/min to completely dissolve rosin, and preparing a rosin mixed solution;
(3) adding 3.5 parts by weight of activated clay, molybdenum and sunflower seed oil into the rosin mixed solution prepared in the step (2) by taking parts by weight as a unit, wherein the weight ratio of the activated clay to the molybdenum to the sunflower seed oil is 14:83:18, then introducing hydrogen, the pressure of the hydrogen is 16MPa, heating to 118 ℃, carrying out addition reaction for 80min, and filtering to remove the activated clay and the molybdenum to prepare a rosin mixture;
(4) taking parts by weight as a unit, adding 40 parts of 2, 2-dimethyl-1, 3-propylene glycol into the rosin mixture prepared in the step (3), adding 4 parts by weight of vanadium pentoxide and diatomite in a weight ratio of 9:2.3, carrying out esterification reaction at 275 ℃ for 1.2h, and filtering to remove the vanadium pentoxide and the diatomite to prepare a rosin resin semi-finished product;
(5) and (3) after cooling, adding 13 parts by weight of fatty alcohol-polyoxyethylene ether sodium sulfate into the rosin resin semi-finished product prepared in the step (4), keeping the temperature at 108 ℃ for 53min, discharging and cooling to prepare the light-color high-stability water-soluble rosin resin.
Comparative example 1
The process for preparing water-soluble rosin resin of example 2 was substantially the same except that activated clay, molybdenum and sunflower seed oil were absent in step (2).
Comparative example 2
The process for preparing a water-soluble rosin resin was substantially the same as that of example 2, except that activated clay was absent in step (2).
Comparative example 3
The process for preparing a water-soluble rosin resin was substantially the same as that of example 2 except that molybdenum was absent in step (2).
Comparative example 4
The process for preparing water-soluble rosin resin of example 2 was substantially the same except that sunflower seed oil was absent in step (2).
Comparative example 5
The water-soluble rosin resins were prepared by the processes of examples 1 to 5 using the Chinese patent application document "A production method of Water-soluble rosin resins (application publication No. CN 106752966A)".
The performance indexes of the water-soluble rosin resins of examples 1 to 3 and comparative examples 1 to 5 were examined, and each performance index was measured in parallel three times. Wherein the color is detected by a hasen colorimetric method. The rosin resin water solubility test method is as follows: a10 g water-soluble rosin resin sample was weighed in an Erlenmeyer flask, and water was added thereto, and the mixture was shaken and mixed until fine insoluble matter appeared in the mixture or insoluble matter adhered to the inner wall of the Erlenmeyer flask, and the amount of water added was read. The measurements were performed in triplicate and averaged. The water solubility was calculated as: water solubility times (mass (g) of added water)/mass (g) of rosin resin. The results of the performance index measurements are shown in the following table.
From the above table, it can be seen that: (1) as can be seen from the color (Harson color number) and water solubility (multiple) data measured in examples 1-3 and comparative example 5, the water-soluble rosin resin prepared by the invention has obviously lighter color and water solubility than the water-soluble rosin resin prepared by the prior art, obviously higher water solubility, at least 10 Harson color numbers and at least 23 times higher water solubility; after the water-soluble rosin resins of the examples 1-3 and the comparative example 5 are heated at 180 ℃ for 8 hours, the water-soluble rosin resins of the examples 1-3 are detected to have 5-7 haas high in color and 13-21 haas high in color and luster, so that the water-soluble rosin resin prepared by the method has higher stability than the water-soluble rosin resin prepared by the prior art.
(2) As can be seen from the color (hason color number) data measured in example 2 and comparative examples 1 to 4, the activated clay, molybdenum and sunflower seed oil play a synergistic role in the addition reaction, the color of the water-soluble rosin resin is significantly reduced, which is the role of catalytic hydrogenation of molybdenum, the activated clay can make molybdenum adsorb and disperse, the intensity of catalytic hydrogenation of molybdenum is increased, and the sunflower seed oil can play a role in lightening the color of the resin, so that the color of the water-soluble rosin resin is significantly reduced under the synergistic role of the activated clay, molybdenum and sunflower seed oil in the addition reaction.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of light-color high-stability water-soluble rosin resin is characterized by comprising the following steps:
(1) pulverizing rosin to obtain pulverized rosin;
(2) adding 250 parts of 130-250 parts of ethanol into 78-92 parts of the rosin crushed material prepared in the step (1) by weight, and heating under stirring to completely dissolve the rosin to prepare a rosin mixed solution;
(3) adding 2.4-3.6 parts by weight of activated clay, molybdenum and sunflower seed oil into the rosin mixed solution prepared in the step (2) by weight, introducing hydrogen, heating to perform addition reaction for 75-95min, and filtering to remove the activated clay and the molybdenum to prepare a rosin mixture;
(4) taking parts by weight as a unit, adding 25-42 parts of 2, 2-dimethyl-1, 3-propylene glycol into the rosin mixture prepared in the step (3), adding 2.8-4.2 parts of vanadium pentoxide and diatomite by total weight, carrying out esterification reaction at the temperature of 270-275 ℃ for 1.2-1.4h, and filtering to remove the vanadium pentoxide and the diatomite to prepare a rosin resin semi-finished product;
(5) and (3) after cooling, adding 8-15 parts by weight of fatty alcohol-polyoxyethylene ether sodium sulfate into the rosin resin semi-finished product prepared in the step (4), preserving the heat for 40-55min, discharging and cooling to prepare the light-colored high-stability water-soluble rosin resin.
2. The method for preparing the light-colored high-stability water-soluble rosin resin according to claim 1, wherein the mass concentration of ethanol in the step (2) is 85-92%.
3. The method as claimed in claim 1, wherein the stirring speed in step (2) is 100-200 r/min.
4. The method as claimed in claim 1, wherein the temperature in step (2) is raised to 162-167 ℃.
5. The method for preparing the light-colored high-stability water-soluble rosin resin according to claim 1, wherein the weight ratio of the activated clay, the molybdenum and the sunflower seed oil in the step (3) is 7-16:30-85: 9-20.
6. The method for preparing the light-colored high-stability water-soluble rosin resin according to claim 1, wherein the hydrogen pressure in step (3) is 10 to 20 MPa.
7. The method as claimed in claim 1, wherein the temperature in step (3) is increased to 110-120 ℃ for addition reaction.
8. The method for preparing the light-colored high-stability water-soluble rosin resin according to claim 1, wherein the weight ratio of the vanadium pentoxide to the diatomite in the step (4) is 4-9: 1.2-2.3.
9. The method as claimed in claim 1, wherein the temperature of the heat preservation in step (5) is 104-117 ℃.
10. A light-colored, high stability, water soluble rosin resin prepared according to the method of any one of claims 1-9.
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