CN107489064A - A kind of preparation method of the AKD emulsions of activating agent - Google Patents
A kind of preparation method of the AKD emulsions of activating agent Download PDFInfo
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- CN107489064A CN107489064A CN201710740945.0A CN201710740945A CN107489064A CN 107489064 A CN107489064 A CN 107489064A CN 201710740945 A CN201710740945 A CN 201710740945A CN 107489064 A CN107489064 A CN 107489064A
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H19/00—Coated paper; Coating material
- D21H19/36—Coatings with pigments
- D21H19/38—Coatings with pigments characterised by the pigments
- D21H19/40—Coatings with pigments characterised by the pigments siliceous, e.g. clays
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H19/00—Coated paper; Coating material
- D21H19/36—Coatings with pigments
- D21H19/44—Coatings with pigments characterised by the other ingredients, e.g. the binder or dispersing agent
- D21H19/46—Non-macromolecular organic compounds
- D21H19/48—Diolefins, e.g. butadiene; Aromatic vinyl monomers, e.g. styrene; Polymerisable unsaturated acids or derivatives thereof, e.g. acrylic acid
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H19/00—Coated paper; Coating material
- D21H19/36—Coatings with pigments
- D21H19/44—Coatings with pigments characterised by the other ingredients, e.g. the binder or dispersing agent
- D21H19/54—Starch
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H19/00—Coated paper; Coating material
- D21H19/36—Coatings with pigments
- D21H19/44—Coatings with pigments characterised by the other ingredients, e.g. the binder or dispersing agent
- D21H19/64—Inorganic compounds
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
- D21H21/16—Sizing or water-repelling agents
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- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Paper (AREA)
Abstract
The present invention relates to a kind of preparation method of the AKD emulsions of activating agent, comprise the following steps：（1）The preparation of emulsifying agent aqueous phase：Hectorite is soaked with water, is mixed with the aluminium polychloride hydrosol；（2）The preparation of stabilizer aqueous phase：Cationic starch is gelatinized；（3）It is prepared by emulsion：Emulsifying agent aqueous phase is mixed with AKD melt liquids, is stirred, is added stabilizer aqueous phase, continue to stir, the O/W type AKD emulsions stablized.The present invention is using aluminium polychloride and nano-solid particle hectorite as emulsifying agent, using cationic starch as stabilizer, emulsifying agent and stabilizer segmentation add, emulsion is made, preparation technology is simple, surfactant is not added, avoids the bubble-related issues that surfactant is brought, stability of emulsion is lasting, liquid-drop diameter is small, and sizing efficiency is good.
Description
Technical field
The present invention relates to a kind of preparation method of AKD emulsions, and in particular to a kind of making side of the AKD emulsions of activating agent
Method.
Background technology
Alkyl ketene dimer（AKD）One of conventional sizing agent of current paper industry neutral-alkaline sizing, be it is a kind of not
Saturation lactone, the waxy solid of water is insoluble under normal temperature, emulsion must be prepared into before.The conventional neutral and alkali of another kind
Glue used in paper-making is alkenyl succinic anhydride（ASA）, it is liquid under normal temperature, having in its molecular structure can interact with cellulose
Acid anhydrides, reactivity is stronger compared with AKD, and it is contacted with water occurs more violent hydrolysis, and its hydrolysate not only without
Sizing efficiency emulsion poor storage stability, can also need plant site to emulsify, limit its extensive use to producing copy paper obstacle.
Lactonic ring hydrolysis rate in AKD molecular structures is slower, is solia particle under emulsion droplet normal temperature, depot good, the good breast of emulsion
Emulsion prepared by chemical industry skill can place 2 ~ 3 months, and sizing efficiency is high, and advantage of lower cost, these advantages promote the extensive of it
Use.AKD emulsions storage period is grown, and in emulsion storing process, emulsion droplets are easily assembled, flocculating causes creaming of emulsion, therefore, with
ASA requires harsher compared to AKD emulsifying process.AKD is usually heated to melt and dissolved by the emulsifying process of AKD emulsions now, so
Cationic starch added afterwards after dispersant, surfactant, gelatinization etc., the emulsifying after premixing, homogeneous terminates rear cold
But tinning.The technique is complex, production cycle length, and the surfactant added in emulsion process can reduce sizing efficiency, hold
Bubble is also easy to produce, brings bubble-related issues to copy paper system, or even produce paper defects.
201410670888.X patent provides a kind of preparation method of the AKD sizing agents of nano micro crystal cellulose, keeps away
The use of Cypres is exempted from, the internal sizing that top sizing can be also used for paper pulp can be carried out, significantly improve page
Degree of sizing, but the preparation method of current microcrystalline cellulose is complex and expensive, is unfavorable for its extensive commercial Application.Specially
Profit number provides a kind of low molecule aminated compounds for ZL200910231301.4 patent and prepares AKD with hectorite jointly stabilizing
The method of emulsion, but the storage stability of emulsion is still needed further raising.In view of AKD widely use and presently, there are ask
Topic, still needs to further study new A KD emulsion technologies of preparing, to prepare sizing efficiency height, adapts to the applying glue of modern paper enterprise
Agent.
The content of the invention
To solve the above problems, the present invention provides a kind of preparation method of the AKD emulsions of activating agent, this method avoid table
The use of face activating agent, good emulsion stability, storage is good, and preparation technology is simple, and sizing efficiency is good.
The present invention is achieved by the following technical solutions：
The preparation method of the AKD emulsions of a kind of activating agent, it is characterised in that comprise the following steps：
（1）The preparation of emulsifying agent aqueous phase：Hectorite is soaked with deionized water, disperses obtained hectorite colloid, with polyaluminium
The aluminium hydrosol mixes；
（2）The preparation of stabilizer aqueous phase：Cationic starch is fully gelatinized in water；
（3）It is prepared by emulsion：AKD, emulsifying agent aqueous phase, the stabilizer heated aqueous of melting, by emulsifying agent aqueous phase and AKD melt liquids
Mixing, stirs under the mechanism of mulser, adds stabilizer aqueous phase, continue to stir, obtain emulsion, cools down, and obtains stabilization
O/W type AKD emulsions.
It is solid-state form, the various AKD works for paper-making sizing without emulsification under normal temperature that AKD involved in the present invention, which is,
Industry product, its fusing point are generally 45~55 DEG C, and in the market is commercially available.To ensure the active ingredient of glue used in paper-making, AKD and step
（1）With（2）Middle aqueous phase total mass ratio is 1:3~19, preferable ratio is 1:4~9.
Particulate hectorite involved in the present invention is commercially available artificial synthesized hectorite class clay mineral, its structure and group
Into similar with natural hectorite, but purity is high, and monodispersity is good, and single crystalline solid is discoid, 25~30nm of diameter, thickness
About 1nm cation exchange capacity (CEC)s are high, have higher negative electrical charge, are dispersed in water and become colloid.As breast in the present invention
The mass ratio of one of change AKD primary emulsion, hectorite and AKD wax disk(-sc)s is 1:20~200, preferable ratio is 1:40~
100。
Aluminium polychloride involved in the present invention（PAC）Also referred to as aluminium chloride, be between AlCl3 and Al (OH) 3 it
Between a kind of water-soluble inorganic high molecular polymer, be commercially available prod.Aluminium polychloride and AKD mass ratio are 1:40~400,
It is preferably in a proportion of 1:100~200.
Cationic starch involved in the present invention be cornstarch, tapioca or farina be modified the sun that obtains from
Sub- starch, cationic starch and AKD mass ratio are 1:3~20, preferable ratio is 1:4~10.
In the preparation scheme of AKD emulsions involved in the present invention, involved AKD and emulsifier dispersion system are mixed
Mechanical shearing effect can be provided by any one stirring or mechanized clipping equipment, it is desirable to 6000~20000 revs/min of mixing speed
Clock, mixing time 2~15 minutes；Preferable mixing speed is 9000~15000 revs/min, and mixing time is 3~10 minutes,
Enough energy are provided to be dispersed into small oil droplet in water for oily AKD.
Cationic starch stabilizer involved in the present invention is added in the above-mentioned emulsion prepared, using identical equipment machine
Tool stirs, it is desirable to 6000~20000 revs/min of mixing speed, mixing time 2~8 minutes；Preferable mixing speed is 9000~
15000 revs/min, mixing time is 3~5 minutes, to improve emulsion storage stability.
AKD involved in the present invention, emulsifying agent aqueous phase and stabilizer aqueous phase temperature range are 55~85 DEG C, are more highly preferred to
Be 65~75 DEG C.
Beneficial effects of the present invention：
Using aluminium polychloride and nano-solid particle hectorite as emulsifying agent, using cationic starch as stabilizer, breast
Agent and stabilizer segmentation add, and emulsion are made, preparation technology is simple, does not add surfactant, avoids surfactant
The bubble-related issues brought, stability of emulsion is lasting, and liquid-drop diameter is small, and sizing efficiency is good.
Embodiment
Below by embodiment, the present invention will be further elaborated, and the description below is only for explaining the present invention, not
Its content is defined.
Number is mass parts in embodiment.
Embodiment 1
The preparation of emulsifying agent and stabilizer：2 parts of hectorites are scattered in 398 parts of water, 1 part of PAC is scattered in 19 parts of water, will
PAC solution mixes with hectorite homogeneous dispersion is used as emulsifying agent；15 parts of cation cassava starch are gelatinized to work in 265 parts of water
For stabilizer.The two be separately heated to 75 DEG C it is standby.
AKD is emulsified：Weigh industrial goods AKD100 parts to melt at 75 DEG C, the emulsifying agent of above-mentioned preparation is added into melting
In AKD, keep emulsifying temperature be 75 DEG C, using high-speed mixing equipment under 15000 revs/min of rotating speeds stirring and emulsifying 5 minutes, then
75 DEG C of cationic starch dextrin is added, maintains rotating speed to continue emulsification 3 minutes, cooling, obtained AKD emulsions are homogeneous milky white
Color oil-in-water type（O/W）Emulsion.AKD mass percent is about 12.5%, and emulsion particle diameter is 1~2 μm.
Plasm-glue-blending effect：Take 100 parts of poplar bleached chemi-mechanical pulps to be dispersed in 9900 parts of water, after being uniformly dispersed, add
Enter 1 part of above-mentioned AKD emulsion for standing 30 days, 0.03 part of CPAM, 0.3 part of bentonite, paper stock is formed after well mixed, and by fast
Fast kayser method sheet forming apparatus copy formulation amount about 60g/m2 handsheet, utilize Liquid Penetrant method（GB/T5405—2002）Measure
Handsheet degree of sizing is 102s.
Embodiment 2
The preparation of emulsifying agent and stabilizer：5 parts of hectorites are scattered in 145 parts of water, 2.5 parts of PAC are scattered in 7.5 parts of water,
Mixed PAC solution with hectorite dispersion liquid as emulsifying agent；5 parts of cations are etherified into cornstarch to be gelatinized in 135 parts of water
As stabilizer.The two be separately heated to 85 DEG C it is standby.
AKD emulsification：Industrial goods AKD100 parts are weighed, 85 DEG C of meltings, the emulsifying agent of above-mentioned preparation are added to the AKD melted
In, keep emulsifying temperature be 85 DEG C, using high-speed mixing equipment under 20000 revs/min of rotating speeds stirring and emulsifying 10 minutes, then add
Enter 85 DEG C of cationic starch dextrin, maintain rotating speed to continue stirring 8 minutes, cooling, obtained AKD emulsions are homogeneous milky
Oil-in-water type（O/W）Emulsion.AKD mass percent is about 25%, and emulsion particle diameter is 1~3 μm.
Plasm-glue-blending effect：50 parts of poplar bleached chemi-mechanical pulps and 50 parts of Straw Pulp is taken to be dispersed in 9900 parts of water,
After being uniformly dispersed, 0.5 part of above-mentioned AKD emulsion for standing 30 days, 0.03 part of CPAM, 0.3 part of bentonite, shape after being well mixed are added
Into paper stock, and formulation amount about 60g/m2 handsheet is copied by quick kayser method sheet forming apparatus, utilize Liquid Penetrant method（GB/
T5405—2002）It is 82s to measure handsheet degree of sizing.
Embodiment 3
The preparation of emulsifying agent and stabilizer：0.5 part of hectorite is scattered in 299.5 parts of water, 2.5 parts of PAC are scattered in 17.5 parts
In water, mixed PAC solution with hectorite dispersion liquid as emulsifying agent；33.3 parts of cations are etherified into farina to exist
Stabilizer is made in gelatinization in 116.7 parts of water.The two be separately heated to 55 DEG C it is standby.
AKD emulsification：Industrial goods AKD100 parts are weighed, are heated to 55 DEG C of meltings, the emulsifying agent of above-mentioned preparation are added molten
In the AKD melted, it is 55 DEG C to keep emulsifying temperature, and using high-speed mixing equipment, stirring and emulsifying 15 is divided under 10000 revs/min of rotating speeds
Clock, 55 DEG C of cationic starch dextrin is then added, continue emulsification 2 minutes, cooling, obtained AKD emulsions are homogeneous milky white
Color oil-in-water type（O/W）Emulsion.AKD mass percent is about 20%, and emulsion particle diameter is 1~3 μm.
Plasm-glue-blending effect：50 parts of hardwood pulps and 50 parts of softwood pulps are taken to be dispersed in 9900 parts of water, after being uniformly dispersed,
0.6 part of above-mentioned AKD emulsion for standing 30 days, 0.03 part of CPAM are added, 0.3 part of bentonite, paper stock is formed after well mixed, and lead to
The handsheet that quick kayser method sheet forming apparatus copy formulation amount about 60g/m2 is crossed, utilizes Liquid Penetrant method（GB/T5405—2002）
It is 86s to measure handsheet degree of sizing.
Embodiment 4
The preparation of emulsifying agent and stabilizer：1 part of hectorite is scattered in 399 parts of water, 0.2 part of PAC is scattered in 19.8 parts of water,
Mixed PAC solution with hectorite dispersion liquid as emulsifying agent.13 share cation etherification starch are gelatinized to work in 327 parts of water
For stabilizer.The two be separately heated to 65 DEG C it is standby.
AKD emulsification：Industrial goods AKD40 parts are weighed, are heated to 65 DEG C of meltings, the emulsifying agent of above-mentioned preparation is added into melting
AKD in, keep emulsifying temperature be 65 DEG C, using high-speed mixing equipment under 15000 revs/min of rotating speeds stirring and emulsifying 2 minutes,
65 DEG C of cationic starch dextrin is then added, maintains rotating speed to continue emulsification 5 minutes, cooling, obtained AKD emulsions are homogeneous
Milky oil-in-water type（O/W）Emulsion.AKD mass percent is about 5%, and emulsion particle diameter is 1~3 μm.
Plasm-glue-blending effect：Take 100 parts of hardwood pulps to be dispersed in 9900 parts of water, after being uniformly dispersed, add and stand 30 days
2 parts of above-mentioned AKD emulsions, 0.03 part of CPAM, 0.3 part of bentonite, paper stock is formed after well mixed, and pass through quick kayser method paper
Page former copies formulation amount about 60g/m2 handsheet, utilizes Liquid Penetrant method（GB/T5405—2002）Measure handsheet applying glue
Spend for 66s.
Embodiment 5
The preparation of emulsifying agent and stabilizer：2.5 parts of hectorites are scattered in 397.5 parts of water, 0.25 part of PAC is scattered in 19.75
In part water, mixed PAC solution with hectorite dispersion liquid as emulsifying agent；25 parts of cationic starches are gelatinized in 455 parts of water
As stabilizer.The two be separately heated to 65 DEG C it is standby.
AKD emulsification：Industrial goods AKD100 parts are weighed, are heated to 65 DEG C of meltings, the emulsifying agent of above-mentioned preparation are added molten
In the AKD melted, it is 65 DEG C to keep emulsifying temperature, and using high-speed mixing equipment, stirring and emulsifying 3 is divided under 9000 revs/min of rotating speeds
Clock, 65 DEG C of cationic starch dextrin is then added, maintain rotating speed to continue emulsification 4 minutes, cooling, obtained AKD emulsions are
Homogeneous milky oil-in-water type（O/W）Emulsion.AKD mass percent is about 10%, and emulsion particle diameter is 1~3 μm.
Plasm-glue-blending effect：100 parts of Straw Pulps are taken to be dispersed in 9900 parts of water, after being uniformly dispersed, addition stands the 1 of 30 days
The above-mentioned AKD emulsions of part, 0.03 part of CPAM, 0.3 part of bentonite, paper stock are formed after well mixed, and pass through quick kayser method page
Former copies formulation amount about 60g/m2 handsheet, utilizes Liquid Penetrant method（GB/T5405—2002）Measure handsheet degree of sizing
For 72s.
Embodiment 6
The preparation of emulsifying agent and stabilizer：1 part of hectorite is scattered in 499 parts of water, 1 part of PAC is scattered in 19 parts of water, will
PAC solution mixes with hectorite dispersion liquid is used as emulsifying agent.10 parts of cation etherification starch are gelatinized as steady in 170 parts of water
Determine agent.The two be separately heated to 80 DEG C it is standby.
AKD emulsification：Industrial goods AKD100 parts are weighed, are heated to 80 DEG C of meltings, the emulsifying agent of above-mentioned preparation are added molten
In the AKD melted, it is 80 DEG C to keep emulsifying temperature, and using high-speed mixing equipment, stirring and emulsifying 10 is divided under 6000 revs/min of rotating speeds
Clock, 80 DEG C of cationic starch dextrin is added, maintain rotating speed to continue emulsification 3 minutes, cooling, obtained AKD emulsions are equal
One milky oil-in-water type（O/W）Emulsion.AKD mass percent is about 12.5%, and emulsion particle diameter is 1~3 μm.
Plasm-glue-blending effect：Take 50 parts of Straw Pulps and 50 parts of softwood pulps to be dispersed in 9900 parts of water, after being uniformly dispersed, add
Enter 1 part of above-mentioned AKD emulsion for standing 30 days, 0.03 part of CPAM, 0.3 part of bentonite, paper stock is formed after well mixed, and by fast
Fast kayser method sheet forming apparatus copy formulation amount about 60g/m2 handsheet, utilize Liquid Penetrant method（GB/T5405—2002）Measure
Handsheet degree of sizing is 81s.
Claims (6)
1. the preparation method of the AKD emulsions of a kind of activating agent, it is characterised in that comprise the following steps：
（1）The preparation of emulsifying agent aqueous phase：Hectorite is soaked with deionized water, disperses obtained hectorite colloid, with polyaluminium
The aluminium hydrosol mixes；
（2）The preparation of stabilizer aqueous phase：Cationic starch is fully gelatinized in water；
（3）It is prepared by emulsion：AKD, emulsifying agent aqueous phase, the stabilizer heated aqueous of melting, by emulsifying agent aqueous phase and AKD melt liquids
Mixing, stirs under the mechanism of mulser, adds stabilizer aqueous phase, continue to stir, obtain emulsion, cools down, and obtains stabilization
O/W type AKD emulsions.
2. the preparation method of the AKD emulsions of a kind of activating agent according to claim 1, it is characterised in that hectorite and AKD
Mass ratio be 1:20~200, aluminium polychloride and AKD mass ratio are 1:40~400, cationic starch and AKD quality
Than for 1:3~20, AKD and step（1）With（2）Middle aqueous phase total mass ratio is 1:3~19.
A kind of 3. preparation method of the AKD emulsions of activating agent according to claim 2, it is characterised in that
Hectorite and AKD mass ratio are 1:40~100；
Aluminium polychloride and AKD mass ratio are 1:100~200；
Cationic starch and AKD mass ratio are 1:4~10；
AKD and step（1）With（2）Middle aqueous phase total mass ratio is 1:4~9.
A kind of 4. preparation method of the AKD emulsions of activating agent according to claim 1, it is characterised in that step（3）In plus
Hot temperature is 55~85 DEG C, 6000~20000 revs/min of mulser mixing speed, mixing time 2~15 minutes；Continue to stir
6000~20000 revs/min of speed, mixing time 2~8 minutes.
A kind of 5. preparation method of the AKD emulsions of activating agent according to claim 4, it is characterised in that step（3）In plus
Hot temperature is 65~75 DEG C, 9000~15000 revs/min of mulser mixing speed, mixing time 3~10 minutes；Continue to stir
9000~15000 revs/min of speed, mixing time 3~5 minutes.
A kind of 6. preparation method of the AKD emulsions of activating agent according to one of claim 1-5, it is characterised in that step
（2）Described cationic starch is that cornstarch, tapioca or farina are modified the cationic starch obtained.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108385434A (en) * | 2018-01-17 | 2018-08-10 | 山东晨鸣纸业集团股份有限公司 | A kind of preparation method of AKD microemulsions |
| CN109403131A (en) * | 2018-09-29 | 2019-03-01 | 青岛科技大学 | A kind of preparation method of AKD lotion |
-
2017
- 2017-08-25 CN CN201710740945.0A patent/CN107489064A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108385434A (en) * | 2018-01-17 | 2018-08-10 | 山东晨鸣纸业集团股份有限公司 | A kind of preparation method of AKD microemulsions |
| CN108385434B (en) * | 2018-01-17 | 2021-03-02 | 山东晨鸣纸业集团股份有限公司 | Preparation method of AKD microemulsion |
| CN109403131A (en) * | 2018-09-29 | 2019-03-01 | 青岛科技大学 | A kind of preparation method of AKD lotion |
| CN109403131B (en) * | 2018-09-29 | 2021-11-02 | 青岛科技大学 | Preparation method of AKD emulsion |
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