CN106118929A - A kind of preparation method of tealeaf residue modification disproportionated rosin potassium soap - Google Patents
A kind of preparation method of tealeaf residue modification disproportionated rosin potassium soap Download PDFInfo
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- CN106118929A CN106118929A CN201610491683.4A CN201610491683A CN106118929A CN 106118929 A CN106118929 A CN 106118929A CN 201610491683 A CN201610491683 A CN 201610491683A CN 106118929 A CN106118929 A CN 106118929A
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- disproportionated rosin
- tealeaf residue
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- potassium soap
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D15/00—Manufacture of resin soap or soaps derived from naphthenic acids; Compositions
Abstract
The invention discloses the preparation method of a kind of tealeaf residue modification disproportionated rosin potassium soap, belong to chemical industry Colophonium deep process technology field.The present invention is with discarded tealeaf residue as raw material, by sucking filtration after pulverizing, obtain filtrate rotary evaporation, prepare concentrated filtrate to mix with disproportionated rosin acyl chlorides, under oil bath is heated, drip methanol, collected by suction filter cake washing with acetone, obtain modified disproportionated rosin, mix with potassium hydroxide stirring, cool down room temperature, thus obtain the preparation method of tealeaf residue modification disproportionated rosin potassium soap.Example proves, present invention process is easy, preparation process more safety and stability, by tannic acid in tealeaf residue and foreign metal complexation in disproportionated rosin, starch conversion adsorption, not only solve the problem that existing disproportionated rosin potassium soap poor transparency, poor heat stability, color number are deep, and and to utilize discarded tealeaf residue be raw material, it is achieved that twice laid, saved cost, emulsion polymerization speed when additionally accelerating rubber production, can be mass-produced application.
Description
Technical field
The invention discloses the preparation method of a kind of tealeaf residue modification disproportionated rosin potassium soap, belong to chemical industry Colophonium deep processing skill
Art field.
Background technology
Disproportionated rosin potassium soap is the kind that in Colophonium deep processed product, yield is bigger, is mainly used as the emulsifying of rubber
Agent, such as, in China Synthetic Rubber Industry, emulsion polymerized styrene butadiene rubber, neoprene, nitrile rubber, ABS and butylbenzene/NBR latex are all used
Disproportionated rosin potassium soap makees emulsifying agent.Using disproportionated rosin to make emulsifying agent can make the cohesive force of rubber strengthen, and high-temperature capability improves, resistance to
Tear strength and tearing toughness are good, and time mixing with natural rubber, adhesive property has greatly improved.
Current domestic disproportionated rosin potassium soap manufacturing enterprise mainly produces the paste of soap product of solid content 60%, 80%.But it is near
Over Nian, client's further requirement provides solid content 25% disproportionated rosin potassium soap aqueous solution.Require that transparency is good, color number is shallow, cloud point
Low, at a temperature of more than 5 DEG C without the solid content 25% disproportionated rosin potassium soap aqueous solution of layering and precipitating.But use solid content at present
The solid content 25% disproportionated rosin potassium soap aqueous solution of 80% paste of soap dilution, pH value to control within 11.3, and cloud point is minimum
Also, between 10～15 DEG C, produce in the winter time and be easy to layering and precipitating after depositing, the color of the most promising improvement product, silicon can be added
The chemical assistants such as acid sodium, but the speed of emulsion polymerization when the existence of sodium silicate can affect rubber production.
It addition, it is first by disproportionated rosin high-temperature digestion that the method for disproportionated rosin potassium soap is prepared by most of producers, then by certain
Potassium hydroxide solution, disproportionated rosin liquid, water are slowly introducing mix homogeneously in reactor by ratio, wherein, it is desirable to potassium hydroxide
Solution adds reactor with disproportionated rosin liquid in strict accordance with certain ratio, and the rate requirement added is the same, adds
Journey need to be stirred continuously.Adopt and prepare disproportionated rosin potassium soap in this way and there is a lot of problem, reality is difficult to control well hydroxide
The addition of potassium solution and disproportionated rosin liquid and add speed, even if use dosing pump is the most not all right.Do not control hydrogen-oxygen well
Changing the addition of potassium solution and disproportionated rosin liquid and add speed, in reactor, whether potassium hydroxide solution is excessive or discrimination
Change Colophonium liquid excess, then the failure of whole preparation process, now reactor can occur high vibration, not only damage equipment, instead
Answer the material in still all to lump and become waste product, not only increase production cost, bring also to the follow-up cleaning of reactor
Great difficulty.
Summary of the invention
The technical problem that present invention mainly solves: for the most conventional disproportionated rosin potassium soap poor transparency, heat stability
Difference, color number are deep, in order to improve product colour, often add the chemical assistants such as sodium silicate, but effect is the most poor, and can affect rubber
The present situation of emulsion polymerization speed during production, it is provided that a kind of with discarded tealeaf residue as raw material, by sucking filtration after pulverizing, obtains filtrate rotation
Turn evaporation, prepare concentrated filtrate and mix with disproportionated rosin acyl chlorides, under oil bath is heated, drip methanol, collected by suction filter cake acetone
Washing, obtains modified disproportionated rosin, mixes with potassium hydroxide stirring, cools down room temperature, thus obtain tealeaf residue modification disproportionated rosin potassium
The preparation method of soap.The method simple process, preparation process more safety and stability, by tannic acid in tealeaf residue and disproportionated rosin
Foreign metal complexation, carries out adsorption by starch conversion, not only solves existing disproportionated rosin potassium soap poor transparency, heat surely
The problem that qualitative difference, color number are deep, and and to utilize discarded tealeaf residue be raw material, it is achieved that twice laid, saved cost, can be big
Large-scale production is applied.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is:
(1) only it is placed in discarded Folium Camelliae sinensis wash heat at 70～80 DEG C being dried 10～12h, chooses dry tealeaf residue and mill and sieve, system
Standby that 80～100 purposes are dried tealeaf residue powder, the most in mass ratio 1:5, tealeaf residue powder is mixed with absolute ethyl alcohol and stirring
Being placed in there-necked flask, under 200～300W, ultrasonic disperse processes after 10～15min, then at 65～80 DEG C of heating in water bath 1～
2h, afterwards sucking filtration collect filtrate, rotate at 65～80 DEG C and be evaporated to the 1/8 of filtrate original volume, be prepared into concentrated filtrate, standby
With；
(2) choose 10～15g corn starchs respectively and 50～80mL pyridines are placed in conical flask, stirring mixing 10～15min
After, conical flask is placed at 100～120 DEG C oil bath activation 10～15min, to be activated complete after, stop heating and also stand cold
But to room temperature；
(3) 1:5 in mass ratio, in the concentrated filtrate prepare disproportionated rosin acyl chlorides interpolation to step (1), stirring is mixed with
Mixed and modified liquid, adds mixed and modified liquid in conical flask subsequently, is continuously heating to 100～120 DEG C, oil bath heating 2～
Being slowly added dropwise 200～230mL methanol after 3h in conical flask, controlling time for adding is 10～15min, after being added dropwise to complete,
Sucking filtration also collects filter cake, after washing with acetone 3～5 times, then is dried 6～8h at 65～80 DEG C, is prepared into modified disproportionated rosin；
(4) choose 30～35mL mass concentration 25% potassium hydroxide solutions to be placed in there-necked flask, heating in water bath to 85～90 DEG C
After, be incubated 10～15min, there-necked flask added the modified disproportionated rosin of 18～20g above-mentioned preparations, stirring is mixed be incorporated in 85～
Heating in water bath at 90 DEG C, detection potassium dehydroabietate mass fraction to be sampled reaches 13%
, stop heating and standing be cooled to room temperature, a kind of tealeaf residue modification disproportionated rosin potassium soap can be prepared into.
The disproportionated rosin potassium soap outward appearance that this law prepares is light succinic acid paste, and cloud point is 2～3 DEG C, and viscosity (30 DEG C) is
5mPa S, freezing point is-5～-DEG C (aqueous solution of 15%), and relative density is 1.2～1.4.
The application process of the present invention is: takes the disproportionated rosin potassium soap that the 100～200g present invention prepare, dilutes with deionized water
5～10 times, afterwards in the production process of butadiene-styrene rubber, it is added thereto to butadiene-styrene rubber quality 1～3% disproportionated rosin potassium soap is dilute
Release liquid, be sufficiently mixed uniformly, emulsion polymeric emulsifiers when producing as butadiene-styrene rubber,.Not only emulsifying effectiveness is good, and
Emulsion polymerization speed when accelerating rubber production, after testing, compared with conventional emulsifier, emulsion polymerization speed can improve 50% with
On.
The invention has the beneficial effects as follows:
(1) present invention is easy and simple to handle, and the discarded tealeaf residue of selection is raw material, it is achieved that twice laid, has saved cost, has decreased
The waste of the energy；
(2) present invention process is easy, and preparation process more safety and stability compared with traditional method, by tannic acid in tealeaf residue and discrimination
Change foreign metal complexation in Colophonium, starch conversion adsorption, solve existing disproportionated rosin potassium soap poor transparency, heat stability
The problem that difference, color number are deep so that prepared disproportionated rosin potassium soap cloud point is only 2～3 DEG C；
(3) present invention not only solves disproportionated rosin potassium soap poor transparency, the deep problem of color number, and newborn when accelerating rubber production
Liquid polymerization speed, can be with large-scale promotion application.
Detailed description of the invention
First only it is placed in discarded Folium Camelliae sinensis wash heat at 70～80 DEG C being dried 10～12h, chooses dry tealeaf residue milled
Sieve, is prepared into 80～100 purposes and is dried tealeaf residue powder, the most in mass ratio 1:5, by tealeaf residue powder and absolute ethyl alcohol and stirring
Mixing is placed in there-necked flask, after under 200～300W, ultrasonic disperse processes 10～15min, then adds 65～80 DEG C of water-baths
Heat 1～2h, afterwards sucking filtration collect filtrate, rotate at 65～80 DEG C and be evaporated to the 1/8 of filtrate original volume, is prepared into concentration filter
Liquid, standby；Choose 10～15g corn starchs the most respectively and 50～80mL pyridines be placed in conical flask, stirring mixing 10～
After 15min, conical flask is placed at 100～120 DEG C oil bath activation 10～15min, to be activated complete after, stop heating the most quiet
Put and be cooled to room temperature；Next 1:5 in mass ratio, adds disproportionated rosin acyl chlorides to above-mentioned prepared concentrated filtrate, stirring
It is mixed with to obtain mixed and modified liquid, subsequently mixed and modified liquid is added to conical flask, be continuously heating to 100～120 DEG C, oil
Being slowly added dropwise 200～230mL methanol after bath heating 2～3h in conical flask, controlling time for adding is 10～15min, waits to drip
After having added, sucking filtration also collects filter cake, after washing with acetone 3～5 times, then is dried 6～8h at 65～80 DEG C, is prepared into modification
Disproportionated rosin；Finally choose 30～35mL mass concentration 25% potassium hydroxide solutions to be placed in there-necked flask, heating in water bath to 85～
After 90 DEG C, being incubated 10～15min, there-necked flask adds the modified disproportionated rosin of 18～20g above-mentioned preparations, stirring is mixed to be incorporated in
Heating in water bath at 85～90 DEG C, detection potassium dehydroabietate mass fraction to be sampled reaches 13%, stops heating and standing is cooled to room
Temperature, can be prepared into a kind of tealeaf residue modification disproportionated rosin potassium soap.
Example 1
First only it is placed in discarded Folium Camelliae sinensis wash heat at 70 DEG C being dried 10h, chooses dry tealeaf residue and mill and sieve, be prepared into 80 mesh
Dry tealeaf residue powder, 1:5 the most in mass ratio, tealeaf residue powder is mixed with absolute ethyl alcohol and stirring and is placed in there-necked flask
In, under 200W, ultrasonic disperse processes after 10min, then at 65 DEG C of heating in water bath 1h, afterwards sucking filtration collect filtrate, at 65 DEG C
Rotary evaporation, to the 1/8 of filtrate original volume, is prepared into concentrated filtrate, standby；Choose 10g corn starch and 50mL pyrrole the most respectively
Pyridine is placed in conical flask, after stirring mixing 10min, conical flask is placed in oil bath activation 10min at 100 DEG C, to be activated complete
Cheng Hou, stops heating and standing is cooled to room temperature；Next 1:5 in mass ratio, adds disproportionated rosin acyl chlorides and prepares to above-mentioned
Concentrated filtrate in, stirring is mixed with to obtain mixed and modified liquid, is added to conical flask by mixed and modified liquid subsequently, continues to rise
Temperature, to 100 DEG C, is slowly added dropwise 200mL methanol in conical flask after oil bath heating 2h, controls time for adding is 10min, treats droplet
After having added, sucking filtration also collects filter cake, after washing with acetone 3 times, then is dried 6h at 65 DEG C, is prepared into modified disproportionated rosin；
Finally choose 30mL mass concentration 25% potassium hydroxide solution to be placed in there-necked flask, after heating in water bath to 85 DEG C, be incubated 10min,
There-necked flask adds the modified disproportionated rosin of the above-mentioned preparation of 18g, and stirring is mixed is incorporated in heating in water bath at 85 DEG C, detection to be sampled
Potassium dehydroabietate mass fraction reaches 13%, stops heating and standing is cooled to room temperature, can be prepared into a kind of tealeaf residue modification disproportionation
Colophonium potash soap.
This example operation is easy, during use, takes the disproportionated rosin potassium soap that the 100g present invention prepares, and dilutes 5 with deionized water
Times, afterwards in the production process of butadiene-styrene rubber, it is added thereto to butadiene-styrene rubber quality 1% disproportionated rosin potassium soap diluent, fills
Point mix homogeneously, emulsion polymeric emulsifiers when producing as butadiene-styrene rubber,.Not only emulsifying effectiveness is good, and accelerates
Emulsion polymerization speed during rubber production, after testing, compared with conventional emulsifier, emulsion polymerization speed can improve 50%.
Example 2
First only it is placed in discarded Folium Camelliae sinensis wash heat at 75 DEG C being dried 11h, chooses dry tealeaf residue and mill and sieve, be prepared into 90 mesh
Dry tealeaf residue powder, 1:5 the most in mass ratio, tealeaf residue powder is mixed with absolute ethyl alcohol and stirring and is placed in there-necked flask
In, under 250W, ultrasonic disperse processes after 13min, then at 75 DEG C of heating in water bath 1.5h, afterwards sucking filtration collect filtrate, at 75 DEG C
Lower rotation is evaporated to the 1/8 of filtrate original volume, is prepared into concentrated filtrate, standby；Choose 13g corn starch and 70mL the most respectively
Pyridine is placed in conical flask, after stirring mixing 13min, conical flask is placed in oil bath activation 13min at 110 DEG C, to be activated
After completing, stop heating and standing is cooled to room temperature；Next 1:5 in mass ratio, adds disproportionated rosin acyl chlorides to above-mentioned system
In the concentrated filtrate obtained, stirring is mixed with to obtain mixed and modified liquid, is added to conical flask by mixed and modified liquid subsequently, continues
Being warming up to 110 DEG C, be slowly added dropwise 220mL methanol in conical flask after oil bath heating 2.5h, control time for adding is 13min,
After being added dropwise to complete, sucking filtration also collects filter cake, after washing with acetone 4 times, then is dried 7h at 75 DEG C, is prepared into modified disproportionation pine
Fragrant；Finally choose 33mL mass concentration 25% potassium hydroxide solution to be placed in there-necked flask, after heating in water bath to 88 DEG C, insulation
13min, adds the modified disproportionated rosin of the above-mentioned preparation of 19g to there-necked flask, and stirring is mixed is incorporated in heating in water bath at 88 DEG C, waits to take
Sample detection potassium dehydroabietate mass fraction reaches 13%, stops heating and standing is cooled to room temperature, can be prepared into a kind of tealeaf residue and change
Property disproportionated rosin potassium soap.
This example operation is easy, during use, takes the disproportionated rosin potassium soap that the 150g present invention prepares, and dilutes 8 with deionized water
Times, afterwards in the production process of butadiene-styrene rubber, it is added thereto to butadiene-styrene rubber quality 2% disproportionated rosin potassium soap diluent, fills
Point mix homogeneously, emulsion polymeric emulsifiers when producing as butadiene-styrene rubber,.Not only emulsifying effectiveness is good, and accelerates
Emulsion polymerization speed during rubber production, after testing, compared with conventional emulsifier, emulsion polymerization speed can improve 52%.
Example 3
First only it is placed in discarded Folium Camelliae sinensis wash heat at 80 DEG C being dried 12h, chooses dry tealeaf residue and mill and sieve, be prepared into 100
Purpose is dried tealeaf residue powder, the most in mass ratio 1:5, is mixed with absolute ethyl alcohol and stirring by tealeaf residue powder and is placed in three mouthfuls of burnings
In Ping, under 300W, ultrasonic disperse processes after 15min, then at 80 DEG C of heating in water bath 2h, afterwards sucking filtration collect filtrate, at 80 DEG C
Lower rotation is evaporated to the 1/8 of filtrate original volume, is prepared into concentrated filtrate, standby；Choose 15g corn starch and 80mL the most respectively
Pyridine is placed in conical flask, after stirring mixing 15min, conical flask is placed in oil bath activation 15min at 120 DEG C, to be activated
After completing, stop heating and standing is cooled to room temperature；Next 1:5 in mass ratio, adds disproportionated rosin acyl chlorides to above-mentioned system
In the concentrated filtrate obtained, stirring is mixed with to obtain mixed and modified liquid, is added to conical flask by mixed and modified liquid subsequently, continues
Being warming up to 120 DEG C, be slowly added dropwise 230mL methanol in conical flask after oil bath heating 3h, control time for adding is 15min, treats
After being added dropwise to complete, sucking filtration also collects filter cake, after washing with acetone 5 times, then is dried 8h at 80 DEG C, is prepared into modified disproportionation pine
Fragrant；Finally choose 35mL mass concentration 25% potassium hydroxide solution to be placed in there-necked flask, after heating in water bath to 90 DEG C, insulation
15min, adds the modified disproportionated rosin of the above-mentioned preparation of 20g to there-necked flask, and stirring is mixed is incorporated in heating in water bath at 90 DEG C, waits to take
Sample detection potassium dehydroabietate mass fraction reaches 13%, stops heating and standing is cooled to room temperature, can be prepared into a kind of tealeaf residue and change
Property disproportionated rosin potassium soap.
This example operation is easy, during use, takes the disproportionated rosin potassium soap that the 200g present invention prepares, and dilutes 10 with deionized water
Times, afterwards in the production process of butadiene-styrene rubber, it is added thereto to butadiene-styrene rubber quality 3% disproportionated rosin potassium soap diluent, fills
Point mix homogeneously, emulsion polymeric emulsifiers when producing as butadiene-styrene rubber,.Not only emulsifying effectiveness is good, and accelerates
Emulsion polymerization speed during rubber production, after testing, compared with conventional emulsifier, emulsion polymerization speed can improve 55%.
Claims (1)
1. the preparation method of a tealeaf residue modification disproportionated rosin potassium soap, it is characterised in that concrete preparation process is:
(1) only it is placed in discarded Folium Camelliae sinensis wash heat at 70～80 DEG C being dried 10～12h, chooses dry tealeaf residue and mill and sieve, system
Standby that 80～100 purposes are dried tealeaf residue powder, the most in mass ratio 1:5, tealeaf residue powder is mixed with absolute ethyl alcohol and stirring
Being placed in there-necked flask, under 200～300W, ultrasonic disperse processes after 10～15min, then at 65～80 DEG C of heating in water bath 1～
2h, afterwards sucking filtration collect filtrate, rotate at 65～80 DEG C and be evaporated to the 1/8 of filtrate original volume, be prepared into concentrated filtrate, standby
With；
(2) choose 10～15g corn starchs respectively and 50～80mL pyridines are placed in conical flask, stirring mixing 10～15min
After, conical flask is placed at 100～120 DEG C oil bath activation 10～15min, to be activated complete after, stop heating and also stand cold
But to room temperature；
(3) 1:5 in mass ratio, in the concentrated filtrate prepare disproportionated rosin acyl chlorides interpolation to step (1), stirring is mixed with
Mixed and modified liquid, adds mixed and modified liquid in conical flask subsequently, is continuously heating to 100～120 DEG C, oil bath heating 2～
Being slowly added dropwise 200～230mL methanol after 3h in conical flask, controlling time for adding is 10～15min, after being added dropwise to complete,
Sucking filtration also collects filter cake, after washing with acetone 3～5 times, then is dried 6～8h at 65～80 DEG C, is prepared into modified disproportionated rosin；
(4) choose 30～35mL mass concentration 25% potassium hydroxide solutions to be placed in there-necked flask, heating in water bath to 85～90 DEG C
After, be incubated 10～15min, there-necked flask added the modified disproportionated rosin of 18～20g above-mentioned preparations, stirring is mixed be incorporated in 85～
Heating in water bath at 90 DEG C, detection potassium dehydroabietate mass fraction to be sampled reaches 13%, stops heating and standing is cooled to room temperature, i.e.
A kind of tealeaf residue modification disproportionated rosin potassium soap can be prepared into.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106978076A (en) * | 2017-03-28 | 2017-07-25 | 常州大学 | A kind of preparation method of high-bond wood wax oil |
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| CN103058857A (en) * | 2013-01-06 | 2013-04-24 | 二创（福建）化工科技有限公司 | Preparation method of disproportionated rosin potassium soap |
| CN104152053A (en) * | 2014-08-26 | 2014-11-19 | 广西众昌树脂有限公司 | Preparation method of disproportionated rosin potash soap |
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| JP2003026954A (en) * | 2001-07-23 | 2003-01-29 | Maruo Calcium Co Ltd | Surface-treated calcium carbonate and sealing composition comprising the same |
| CN103058857A (en) * | 2013-01-06 | 2013-04-24 | 二创（福建）化工科技有限公司 | Preparation method of disproportionated rosin potassium soap |
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| CN106978076A (en) * | 2017-03-28 | 2017-07-25 | 常州大学 | A kind of preparation method of high-bond wood wax oil |
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