CN106496596A - A kind of preparation method of rosin milk - Google Patents
A kind of preparation method of rosin milk Download PDFInfo
- Publication number
- CN106496596A CN106496596A CN201611102072.2A CN201611102072A CN106496596A CN 106496596 A CN106496596 A CN 106496596A CN 201611102072 A CN201611102072 A CN 201611102072A CN 106496596 A CN106496596 A CN 106496596A
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- rosin
- preparation
- rosin milk
- water
- milk
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2393/00—Characterised by the use of natural resins; Derivatives thereof
- C08J2393/04—Rosin
Abstract
The invention discloses a kind of preparation method of rosin milk, using the raw material of following weight portion：8～40 parts of rosin, 7～12 parts of emulsifying agent, 0.1～0.5 part of stabilizer, 45～85 parts of deionized water；Comprise the steps：Emulsifying agent is well mixed with appropriate deionized water, emulsifier solution is configured to；By rosin heating to melting completely, temperature control is subsequently adding emulsifier solution at 100～130 DEG C, emulsified in 400～1000rpm mixing speeds, and emulsification times are 15～30min, make rosin milk System forming water-in-oil type；Boiling water is added dropwise, reaction temperature is controlled at 80～100 DEG C, makes rosin milk system phase inversion form oil-in-water type；Remaining boiling water and stabilizer is rapidly added, is reduced mixing speed and is quickly cooled to less than 20～40 DEG C；Screen filtration, obtains rosin milk finished product.The preparation method of the rosin milk that the present invention is provided is simple to operate, environmental protection, requires relatively low, reduction production cost, obtained rosin milk good water solubility to equipment and operating condition.
Description
Technical field
The present invention relates to rosin deep process technology field, and in particular to a kind of preparation method of rosin milk.
Background technology
Rosin is a kind of reproducible mixing natural resin, is one of most important product in China's forest chemical.At present
Rosin is widely used in industrial production as modifying agent and additive, and this is closely related with its chemical constitution.Due to
It is rotten that the particularity of rosin structure occurs its easy crystallization and oxidation during production, storage and use, so usual will
Rosin carries out deep processing.Both at home and abroad for the deep processing research of rosin is always focus.Wherein, rosin is emulsified using emulsifying agent
Prepared rosin milk is one of hot research.
Rosin milk can be matched with the water-based system in numerous applications and is widely used, for example, adhesive row
Industry, paper-making industry, coating industry and ink industry etc..With developing rapidly for water-base cement and water paint, no matter rosin milk exists
Modified adhesive still has good development and application prospect improving the fields such as coating property.Rosin milk in the market
Product is mainly modified rosin emulsion, but its cost of material is higher, and complicated process of preparation is higher to equipment requirement, partially modified
The solvent of rosin milk is larger to human body and environmental hazard.
The technique that rosin milk is prepared using emulsifying agent has multiple, and conventional mainly have solvent method, high pressure melting method and super
Sound emulsion process.For solvent method, containing harmful organic solvent in obtained rosin milk, rosin is not only limit
The use range of emulsion also needs to carry out taking back and process to solvent.For high pressure melting method and supersound method, preparing
Not only equipment and operating condition are required in journey higher and costly.
Content of the invention
The purpose of the present invention is to overcome above-mentioned technical problem, there is provided a kind of low cost, simple to operate, good water solubility, nontoxic
The preparation method of harmless rosin milk.
Technical scheme is as follows：
A kind of preparation method of rosin milk, using the raw material of following weight portion：
8～40 parts of rosin, 7～12 parts of emulsifying agent, 0.1～0.5 part of stabilizer, 45～85 parts of deionized water；
Comprise the steps：
Step S1, emulsifying agent is well mixed with appropriate deionized water, is configured to emulsifier solution；
Step S2, by rosin heating to melting completely, temperature control is subsequently adding emulsifier solution at 100～130 DEG C,
Emulsified in 400～1000rpm mixing speeds, emulsification times are 15～30min, make rosin milk System forming water-in-oil type；
Step S3, in rosin milk obtained in step S2 be added dropwise boiling water, reaction temperature control at 80～100 DEG C, make pine
Fragrant emulsion system phase inversion forms oil-in-water type；
Step S4, remaining boiling water and stabilizer is rapidly added in rosin milk obtained in step S3, reduce stirring speed
Spend and be quickly cooled to less than 20～40 DEG C；
Step S5, screen filtration, obtain rosin milk finished product.
Preferably, the emulsifying agent is composite emulsifier, its by anion emulsifier and nonionic emulsifier in mass ratio
1:4～6 compositions.
Preferably, the anion emulsifier is the one kind or two in lauryl sodium sulfate and neopelex
Kind, the nonionic emulsifier is Span-80.
Preferably, the stabilizer is polyvinyl alcohol.
Preferably, in obtained rosin milk finished product, the content of rosin is 20～50%.
Preferably, in step S5, the mesh number of screen cloth is 100～400 mesh.
Preferably, the weight of the deionized water in the raw material includes preparing the deionized water and two needed for emulsifier solution
The boiling water of secondary addition.
Preferably, in step S3, the addition of boiling water accounts for the 10～20% of ion water inventory.
Preferably, the preparation method of the rosin milk is carried out at ambient pressure.
Preferably, the rosin in the raw material is natural rosin.
The preparation method of the rosin milk provided compared to prior art, the present invention has the advantages that：
First, the preparation method that the present invention is provided, simple to operate, replaces conventional organic solvents with water, it is to avoid organic solvent
Harm to air and human body, environmental protection；
2nd, carry out at ambient pressure, relatively low, reduction production cost is required to equipment and operating condition；
3rd, composite emulsifier is utilized, improves the emulsifying capacity and utilization rate of emulsifying agent；
4th, with natural rosin as raw material, deep processing is carried out to natural rosin directly, overcomes the perishable defect of rosin,
The field of rosin deep processing has been widened, cost of material has been reduced；
5th, rosin milk good water solubility obtained in the present invention.
Specific embodiment
With reference to embodiment, the present invention is described in further detail, but embodiments of the present invention not limited to this.
Embodiment 1
The preparation method of this rosin milk comprises the steps：
Step S1, emulsifying agent (2.0g lauryl sodium sulfate and 11.0gSpan-80) is mixed with 10g deionized waters
Even, it is configured to emulsifier solution；
Step S2, it is heated to melting completely by 20g rosin (natural masson pine rosin, Jiangxi produce), temperature control is 120
DEG C, emulsifier solution is subsequently adding, emulsified in 800rpm mixing speeds, emulsification times are 20～30min, make rosin milk body
System forms water-in-oil type；
Step S3, in rosin milk obtained in step S2 be added dropwise 10g boiling water, reaction temperature control at 95 DEG C, make rosin
Emulsion system phase inversion forms oil-in-water type；
Step S4,50g boiling water and 0.1g stabilizers (polyvinyl alcohol) is rapidly added in rosin milk obtained in step S3,
Reduce mixing speed and to 200rpm and be quickly cooled to less than 30～40 DEG C；
Step S5,400 mesh sieve net filtrations, obtain rosin milk finished product, the rosin containing 30% in the rosin milk finished product.
Embodiment 2
The preparation method of this rosin milk comprises the steps：
Step S1, emulsifying agent (1.5g lauryl sodium sulfate and 7.5gSpan-80) is mixed with 10g deionized waters
Even, it is configured to emulsifier solution；
Step S2, it is heated to melting completely by 20g rosin (natural bioremediation is loosely fragrant, Jiangxi produce), temperature control is 130
DEG C, emulsifier solution is subsequently adding, emulsified in 600rpm mixing speeds, emulsification times are 20～30min, make rosin milk body
System forms water-in-oil type；
Step S3, in rosin milk obtained in step S2 be added dropwise 10g boiling water, reaction temperature control at 90 DEG C, make rosin
Emulsion system phase inversion forms oil-in-water type；
Step S4,40g boiling water and 0.1g stabilizers (polyvinyl alcohol) is rapidly added in rosin milk obtained in step S3,
Reduce mixing speed and to 200rpm and be quickly cooled to less than 30～40 DEG C；
Step S5,400 mesh sieve net filtrations, obtain rosin milk finished product, the rosin containing 35% in the rosin milk finished product.
Embodiment 3
The preparation method of this rosin milk comprises the steps：
Step S1, emulsifying agent (1.5g lauryl sodium sulfate and 7.5gSpan-80) is mixed with 10g deionized waters
Even, it is configured to emulsifier solution；
Step S2, it is heated to melting completely by 20g rosin (natural masson pine rosin, Hunan produce), temperature control is 110
DEG C, emulsifier solution is subsequently adding, emulsified in 700rpm mixing speeds, emulsification times are 20～30min, make rosin milk body
System forms water-in-oil type；
Step S3, in rosin milk obtained in step S2 be added dropwise 10g boiling water, reaction temperature control at 93 DEG C, make rosin
Emulsion system phase inversion forms oil-in-water type；
Step S4,50g boiling water and 0.15g stabilizer (polyethylene is rapidly added in rosin milk obtained in step S3
Alcohol), reduce mixing speed and to 200rpm and be quickly cooled to less than 30～40 DEG C；
Step S5,400 mesh sieve net filtrations, obtain rosin milk finished product, the rosin containing 28% in the rosin milk finished product.
The performance of rosin milk prepared by embodiment 1-3 is tested, is added dropwise in water respectively, rapidly and water
Dissolve each other, illustrate that obtained rosin milk water solubility is fabulous.
The preparation method of the rosin milk provided compared to prior art, the present invention has the advantages that：
First, the preparation method that the present invention is provided, simple to operate, replaces conventional organic solvents with water, it is to avoid organic solvent
Harm to air and human body, environmental protection；
2nd, carry out at ambient pressure, relatively low, reduction production cost is required to equipment and operating condition；
3rd, composite emulsifier is utilized, improves the emulsifying capacity and utilization rate of emulsifying agent；
4th, with natural rosin as raw material, deep processing is carried out to natural rosin directly, overcomes the perishable defect of rosin,
The field of rosin deep processing has been widened, cost of material has been reduced；
5th, rosin milk good water solubility obtained in the present invention.
Embodiments of the invention are the foregoing is only, the scope of the claims of the present invention is not thereby limited, every using this
Equivalent structure or equivalent flow conversion that bright description is made, or directly or indirectly it is used in other related technology necks
Domain, is included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of rosin milk, it is characterised in that
Raw material using following weight portion：
8～40 parts of rosin, 7～12 parts of emulsifying agent, 0.1～0.5 part of stabilizer, 45～85 parts of deionized water；
Comprise the steps：
Step S1, emulsifying agent is well mixed with appropriate deionized water, is configured to emulsifier solution；
Step S2, by rosin heating to melting completely, temperature control is subsequently adding emulsifier solution at 100～130 DEG C, 400
～1000rpm mixing speeds are emulsified, and emulsification times are 15～30min, make rosin milk System forming water-in-oil type；
Step S3, in rosin milk obtained in step S2 be added dropwise boiling water, reaction temperature control at 80～100 DEG C, make rosin breast
Liquid system phase inversion forms oil-in-water type；
Step S4, remaining boiling water and stabilizer is rapidly added in rosin milk obtained in step S3, reduce mixing speed simultaneously
It is quickly cooled to less than 20～40 DEG C；
Step S5, screen filtration, obtain rosin milk finished product.
2. the preparation method of rosin milk according to claim 1, it is characterised in that the emulsifying agent is compound emulsion
Agent, which is by anion emulsifier and nonionic emulsifier in mass ratio 1:4～6 compositions.
3. the preparation method of rosin milk according to claim 2, it is characterised in that the anion emulsifier is 12
One or two in sodium alkyl sulfate and neopelex, the nonionic emulsifier are Span-80.
4. the preparation method of rosin milk according to claim 1, it is characterised in that the stabilizer is polyvinyl alcohol.
5. the preparation method of rosin milk according to claim 1, it is characterised in that in obtained rosin milk finished product
The content of rosin is 20～50%.
6. the preparation method of rosin milk according to claim 1, it is characterised in that in step S5, the mesh number of screen cloth is
100～400 mesh.
7. the preparation method of rosin milk according to claim 1, it is characterised in that the deionized water bag in the raw material
Include the deionized water needed for preparation emulsifier solution and the boiling water for adding twice.
8. the preparation method of rosin milk according to claim 7, it is characterised in that in step S3, the addition of boiling water
Account for the 10～20% of ion water inventory.
9. the preparation method of the rosin milk according to any one of claim 1-8, it is characterised in that the rosin milk
Preparation method is carried out at ambient pressure.
10. the preparation method of rosin milk according to claim 1, it is characterised in that the rosin in the raw material is day
Right rosin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611102072.2A CN106496596A (en) | 2016-12-05 | 2016-12-05 | A kind of preparation method of rosin milk |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611102072.2A CN106496596A (en) | 2016-12-05 | 2016-12-05 | A kind of preparation method of rosin milk |
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| CN106496596A true CN106496596A (en) | 2017-03-15 |
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| CN201611102072.2A Pending CN106496596A (en) | 2016-12-05 | 2016-12-05 | A kind of preparation method of rosin milk |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107090223A (en) * | 2017-05-26 | 2017-08-25 | 湘潭大学 | Rosin/styrene-acrylic composite emulsion and preparation method thereof, application |
| CN109721676A (en) * | 2018-12-07 | 2019-05-07 | 江阴美源实业有限公司 | A kind of emulsion acrylate class adhesive and preparation method thereof |
| CN111072830A (en) * | 2019-12-31 | 2020-04-28 | 黎月清 | Preparation method of phellandrene resin emulsion |
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|---|---|---|---|---|
| CN1168912A (en) * | 1996-06-14 | 1997-12-31 | 安徽省化工研究院 | Temp. phase transformation art for all-free dispersion rosin size |
| CN1276402A (en) * | 2000-06-24 | 2000-12-13 | 安徽省化工研究院 | Temp phase-transfer process of full-free dispersed rosin size |
| CN102010602A (en) * | 2010-09-30 | 2011-04-13 | 江西金安林产实业有限公司 | Water-based tackifier resin emulsion and preparation method thereof |
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2016
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| CN1168912A (en) * | 1996-06-14 | 1997-12-31 | 安徽省化工研究院 | Temp. phase transformation art for all-free dispersion rosin size |
| CN1276402A (en) * | 2000-06-24 | 2000-12-13 | 安徽省化工研究院 | Temp phase-transfer process of full-free dispersed rosin size |
| CN102010602A (en) * | 2010-09-30 | 2011-04-13 | 江西金安林产实业有限公司 | Water-based tackifier resin emulsion and preparation method thereof |
| CN102911376A (en) * | 2012-11-15 | 2013-02-06 | 广西梧州日成林产化工股份有限公司 | Preparation method of water-based rosin resin tackifying emulsion |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107090223A (en) * | 2017-05-26 | 2017-08-25 | 湘潭大学 | Rosin/styrene-acrylic composite emulsion and preparation method thereof, application |
| CN107090223B (en) * | 2017-05-26 | 2020-06-09 | 湘潭大学 | Rosin/styrene-acrylic composite emulsion and preparation method and application thereof |
| CN109721676A (en) * | 2018-12-07 | 2019-05-07 | 江阴美源实业有限公司 | A kind of emulsion acrylate class adhesive and preparation method thereof |
| CN109721676B (en) * | 2018-12-07 | 2021-05-25 | 江阴美源实业有限公司 | Emulsion type acrylate adhesive and preparation method thereof |
| CN111072830A (en) * | 2019-12-31 | 2020-04-28 | 黎月清 | Preparation method of phellandrene resin emulsion |
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Application publication date: 20170315 |