CN105908567A - Method for preparing alkyl ketene dimer emulsion without surfactants - Google Patents

Method for preparing alkyl ketene dimer emulsion without surfactants Download PDF

Info

Publication number
CN105908567A
CN105908567A CN201610263090.2A CN201610263090A CN105908567A CN 105908567 A CN105908567 A CN 105908567A CN 201610263090 A CN201610263090 A CN 201610263090A CN 105908567 A CN105908567 A CN 105908567A
Authority
CN
China
Prior art keywords
ketene dimer
alkyl ketene
emulsion
preparation
stabilizer
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201610263090.2A
Other languages
Chinese (zh)
Other versions
CN105908567B (en
Inventor
王慧丽
陈学帅
刘温霞
于得海
宋兆萍
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
SHANDONG XILAI STARCH Co.,Ltd.
Original Assignee
Qilu University of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Qilu University of Technology filed Critical Qilu University of Technology
Priority to CN201610263090.2A priority Critical patent/CN105908567B/en
Publication of CN105908567A publication Critical patent/CN105908567A/en
Application granted granted Critical
Publication of CN105908567B publication Critical patent/CN105908567B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP 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
    • D21H21/00Non-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
    • D21H21/14Non-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
    • D21H21/16Sizing or water-repelling agents
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP 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
    • D21H17/00Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/03Non-macromolecular organic compounds
    • D21H17/05Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
    • D21H17/14Carboxylic acids; Derivatives thereof
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP 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
    • D21H17/00Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/03Non-macromolecular organic compounds
    • D21H17/05Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
    • D21H17/17Ketenes, e.g. ketene dimers
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP 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
    • D21H17/00Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/20Macromolecular organic compounds
    • D21H17/21Macromolecular organic compounds of natural origin; Derivatives thereof
    • D21H17/24Polysaccharides
    • D21H17/28Starch
    • D21H17/29Starch cationic
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP 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
    • D21H17/00Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/63Inorganic compounds
    • D21H17/67Water-insoluble compounds, e.g. fillers, pigments
    • D21H17/68Water-insoluble compounds, e.g. fillers, pigments siliceous, e.g. clays
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP 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
    • D21H17/00Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/63Inorganic compounds
    • D21H17/67Water-insoluble compounds, e.g. fillers, pigments
    • D21H17/69Water-insoluble compounds, e.g. fillers, pigments modified, e.g. by association with other compositions prior to incorporation in the pulp or paper

Landscapes

  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Paper (AREA)

Abstract

The invention relates to a method for preparing alkyl ketene dimer emulsion without surfactants. The method includes steps of (1), preparing emulsifier water phases, to be more specific, wetting hectorite, uniformly mixing the hectorite and aqueous solution of water-soluble sodium amino acid salt with each other and regulating pH (potential of hydrogen) values of the hectorite and the aqueous solution by the aid of diluted acid; (2), pasting cationic starch to prepare stabilizer water phases; (3), preparing the alkyl ketene dimer emulsion, to be more specific, mixing the emulsifier water phases and AKD (alkyl ketene dimer) melted liquid with one another to obtain mixtures, stirring the mixtures, adding the stabilizer water phases into the mixtures and continuing to stir the mixtures and the stabilizer water phases to obtain the stable O/W (oil-in-water) type AKD emulsion. The method has the advantages that the water-soluble sodium amino acid salt and the nanometer solid granular hectorite are used as emulsifiers, the cationic starch is used as a stabilizer, the emulsifiers and the stabilizer are added in a sectional manner to prepare the alkyl ketene dimer emulsion, processes for preparing the alkyl ketene dimer emulsion are simple, the surfactants are omitted, accordingly, the problem of foam due to the surfactants can be solved, the alkyl ketene dimer emulsion is durable in stability, liquid drop has a small diameter, and good adhesive application effects can be realized.

Description

A kind of preparation method of surfactant-free alkyl ketene dimer emulsion
Technical field
The present invention relates to the preparation method of a kind of alkyl ketene dimer emulsion, be specifically related to the preparation method of a kind of surfactant-free alkyl ketene dimer emulsion.
Background technology
Alkyl ketene dimer (AKD) is a kind of unsaturated lactone, is insoluble in the waxy solid of water, can be used as glue used in paper-making, but must be prepared as emulsion before use under room temperature, is one of sizing agent that current paper industry neutral-alkaline sizing is conventional.Being liquid under another kind of conventional glue used in paper-making alkenyl succinic anhydride room temperature, the anhydride in its molecular structure easily hydrolyzes, poor storage stability, needs plant site emulsifying, and its hydrolyzate easily deposits on paper machine and causes copy paper obstacle, and its application is by a definite limitation.Lactonic ring hydrolysis rate in alkyl ketene dimer emulsion is relatively slow, and is solid particle under emulsion droplet room temperature, and emulsion is depot good, emulsion prepared by good emulsifying process can place 2 ~ 3 months, sizing efficiency is high, and advantage of lower cost, these advantages promote being widely used of it.But from the point of view of comparing alkenyl succinic anhydride, alkyl ketene dimer emulsion has the requirement of storage property, it is desirable to emulsion to have the performances such as permanent anti-emulsion droplet gathering, and its emulsifying process requires harsher.The emulsifying process of alkyl ketene dimer is usually heated to melt and dissolved now, it is subsequently adding the cationic starch etc. after dispersant, surfactant, gelatinizing, emulsifying after premixing, homogenizing cools down tinning after terminating, this technique is complex, and the production cycle is long.The surfactant added in emulsion process can reduce sizing efficiency, easily produces bubble, brings bubble-related issues to copy paper system, even produces paper defects.Therefore, develop efficient alkyl ketene dimer emulsification system, reduce dosage of surfactant even without surfactant beneficially raising alkyl ketene dimer sizing efficiency, the needs of adaptation papermaking enterprise production and the requirement of green production now.
The patent of Publication No. CN 104499361 provides the preparation method of the alkyl ketene dimer sizing agent of a kind of nano micro crystal cellulose, avoid the use of Cypres, top sizing can be carried out and can be also used for the internal sizing of paper pulp, but the preparation method of microcrystalline Cellulose is complex and expensive at present, is unfavorable for its commercial Application widely.The patent disclosure of Publication No. CN 103774496 a kind of glutamic acid, brucite, the AKD emulsion of diallyl dimethyl ammoniumchloride jointly stabilizing, publication is mentioned the independent glutamic acid alkyl ketene dimer emulsion stable with brucite unstable, the good emulsion stability formed after adding diallyl dimethyl ammoniumchloride, still employs the organic high molecular compound with surface-active action in its emulsion preparation process.The patent of Patent No. ZL 201010281410.X discloses a kind of chitosan and the method for nano titanium oxide associating emulsifying alkyl ketene dimer, emulsifying process is simple, alkyl ketene dimer emulsion sizing efficiency is high, and ripening speed is fast, but emulsion droplets aggregation stability still has much room for improvement.In view of the problem being widely used and presently, there are of alkyl ketene dimer, still need to study Novel alkyl ketene dimer emulsion technology of preparing further, high to prepare sizing efficiency, adapt to the sizing agent of modern paper enterprise.
Summary of the invention
For solving the problems referred to above, the present invention provides the preparation method of a kind of surfactant-free alkyl ketene dimer emulsion, this method avoid the use of surfactant, good emulsion stability, and storage property 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 a kind of surfactant-free alkyl ketene dimer emulsion, it is characterised in that comprise the following steps:
(1) preparation of emulsifying agent aqueous phase: hectorite is used deionized water moistening, dispersion prepare hectorite colloid, uniformly mix with the aqueous solution of water soluble amino acid sodium-salt, be 3~7 with dilute acid for adjusting pH value;
(2) preparation of stabilizer aqueous phase: by cationic starch abundant gelatinizing in water;
(3) prepared by emulsion: melted alkyl ketene dimer, emulsifying agent aqueous phase, stabilizer heated aqueous, by emulsifying agent aqueous phase and melted alkyl ketene dimer liquid mixing, stir under the mechanism of mulser, add stabilizer aqueous phase, continue stirring, obtain emulsion, cooling, obtain stable O/W type alkyl ketene dimer emulsion.
Alkyl ketene dimer involved in the present invention is that its fusing point is generally 45-55 DEG C, commercially available on market for solid-state form, various alkyl ketene dimer industrial products for paper-making sizing without emulsifying under room temperature.For ensureing the effective ingredient of glue used in paper-making, alkyl ketene dimer is 1:3~19 with the total mass ratio of aqueous phase in step (1) and (2), and preferred ratio is 1:4~9.
The Strese Hofmann's hectorite. class clay mineral that solid particle hectorite is commercially available synthetic involved by invention, its structure and composition is similar with natural hectorite, but purity is high, and monodispersity is good, particle diameter is far smaller than common montmorillonite, single crystalline solid is discoid, diameter 25~30nm, and thickness is about 1nm, its cation exchange capacity (CEC) is high, specific surface area is big, and has higher negative charge, is dispersed in water and becomes colloid.As one of the primary emulsion of emulsifying alkyl ketene dimer in the present invention, hectorite is 1:20~200 with the mass ratio of alkyl ketene dimer wax disk(-sc), and preferred ratio is 1:40~100.
Amino acid sodium involved in the present invention includes the water soluble amino acid sodium-salt such as sodium glutamate or NaAsp, and sodium glutamate is also referred to as MSG or monosodium glutamate, is the sodium salt of a kind of glutamic acid.Sodium glutamate structural formula is HOOCCHNH2(CH2)2COONa, the structural formula of NaAsp is HOOCCH2CH(NH2) both COONa structure is closely similar, NaAsp can be used as the antistaling agent of food service industry, preservative, replaces monosodium glutamate.Amino acid sodium is 1:20~400 with the mass ratio of alkyl ketene dimer, is preferably in a proportion of 1:50~200.
Cationic starch involved in the present invention, the cationic starch obtained for corn starch, tapioca or potato starch modification, cationic starch is 1:3~20 with the mass ratio of alkyl ketene dimer, and preferred ratio is 1:4~10.
Described diluted acid is one or more in acetic acid, hydrochloric acid, sulphuric acid and citric acid etc., and suitable emulsifying agent aqueous pH values scope is 3~7, and preferred pH value is 3.5~5.5.
In the preparation scheme of alkyl ketene dimer emulsion involved in the present invention, involved alkyl ketene dimer and the mixed mechanical shearing effect of emulsifier dispersion system can be stirred by any one or mechanized clipping equipment provides, require mixing speed 6000~20000 revs/min, mixing time 2~15 minutes;Preferably scheme is mixing speed 9000~15000 revs/min, and mixing time 3~10 minutes think that oily alkyl ketene dimer is dispersed into the energy that little oil droplet provides enough in water.
Cationic starch stabilizer involved in the present invention joins in the above-mentioned emulsion prepared, and uses identical device mechanical agitation, it is desirable to mixing speed 6000~20000 revs/min, mixing time 2~8 minutes;Preferably scheme is 9000~15000 revs/min, and mixing time is 3~5 minutes, to improve emulsion storage stability.
The temperature range of alkyl ketene dimer, emulsifying agent aqueous phase and stabilizer aqueous phase involved in the present invention is 55~85 DEG C, it is more preferred to 65~75 DEG C.
Beneficial effects of the present invention:
Use water soluble amino acid sodium-salt and nano-solid granule hectorite as emulsifying agent, use cationic starch as stabilizer, emulsifying agent adds with stabilizer segmentation, make emulsion, preparation technology is simple, without surfactant, it is to avoid the bubble-related issues that surfactant brings, stability of emulsion is lasting, liquid-drop diameter is little, and sizing efficiency is good.
Detailed description of the invention
Below by embodiment, the present invention will be further elaborated, and its content, only for explaining the present invention, is not defined by the description below.In embodiment, number is weight portion.
Embodiment 1
Emulsifying agent and the preparation of stabilizer: be scattered in 398 parts of water by 2 parts of hectorites, 1 part of sodium glutamate is scattered in 19 parts of water, is uniformly mixed by two kinds of solution, is 4 with salt acid for adjusting pH value;Using 10 parts of cation cassava starch in 270 parts of water gelatinizing as stabilizer.The two be separately heated to 75 DEG C standby.
AKD emulsifying: weigh industrial goods AKD 100 parts melted at 75 DEG C, the emulsifying agent of above-mentioned preparation is added in melted AKD, keeping emulsifying temperature is 75 DEG C, utilize high-speed mixing equipment stirring and emulsifying 8 minutes under 10000 revs/min of rotating speeds, add the cationic starch dextrin of 75 DEG C, maintaining rotating speed to continue emulsifying 3 minutes, cooling, the AKD emulsion prepared is homogeneous milky oil-in-water type (O/W) emulsion.The mass percent of AKD 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 and be dispersed in 9900 parts of water, after being uniformly dispersed, add the 1 part of above-mentioned AKD emulsion standing 30 days, 0.03 part of CPAM, 0.3 part of bentonite, form paper stock after mix homogeneously, and copy formulation by quick kayser method sheet forming apparatus and measure about 60g/m2Handsheet, utilizing liquid infiltration method (GB/T5405 2002) to record handsheet degree of sizing is 86s.
Embodiment 2
Emulsifying agent and the preparation of stabilizer: be scattered in 398 parts of water by 2 parts of hectorites, 0.25 part of sodium glutamate is scattered in 20 parts of water, is sufficiently mixed by two kinds of solution, is 3 with sulfur acid for adjusting pH value;Using 25 parts of cationes etherificate corn starchs in 255 parts of water gelatinizing as stabilizer.The two be separately heated to 55 DEG C standby.
The emulsifying of AKD: weigh industrial goods AKD 100 parts, 55 DEG C melt, the emulsifying agent of above-mentioned preparation is added in melted AKD, keeping emulsifying temperature is 55 DEG C, utilize high-speed mixing equipment stirring and emulsifying 2 minutes under 15000 revs/min of rotating speeds, add the cationic starch dextrin of 55 DEG C, maintain rotating speed to continue stirring 5 minutes, cooling, the AKD emulsion prepared is homogeneous milky oil-in-water type (O/W) emulsion.The mass percent of AKD is about 12.5%, and emulsion particle diameter is 1~3 μm.
Plasm-glue-blending effect: take 100 parts of poplar chemi-mechanical pulps and be dispersed in 9900 parts of water, after being uniformly dispersed, add the 1 part of above-mentioned AKD emulsion standing 30 days, 0.03 part of CPAM, 0.3 part of bentonite, form paper stock after mix homogeneously, and copy formulation by quick kayser method sheet forming apparatus and measure about 60g/m2Handsheet, utilizing liquid infiltration method (GB/T5405 2002) to record handsheet degree of sizing is 56s.
Embodiment 3
Emulsifying agent and the preparation of stabilizer: be scattered in 145 parts of water by 5 parts of hectorites, 2 parts of sodium glutamate are scattered in 8 parts of water, are sufficiently mixed by two kinds of solution, are 7 with salt acid for adjusting pH value;Stabilizer is made in the gelatinizing in 135 parts of water of 5 parts of cationic potato starch.The two be separately heated to 85 DEG C standby.
The emulsifying of AKD: weigh industrial goods AKD 100 parts, it is heated to 85 DEG C melt, the emulsifying agent of above-mentioned preparation is added in melted AKD, keeping emulsifying temperature is 85 DEG C, utilize high-speed mixing equipment stirring and emulsifying 10 minutes under 20000 revs/min of rotating speeds, being subsequently added the cationic starch dextrin of 85 DEG C, continue emulsifying 8 minutes, the AKD emulsion prepared is homogeneous milky oil-in-water type (O/W) emulsion.The mass percent of AKD is about 25%, and emulsion particle diameter is 1~3 μm.
Plasm-glue-blending effect: take 50 parts of hardwood pulps and 50 parts of softwood pulps are dispersed in 9900 parts of water, after being uniformly dispersed, add the 0.5 part of above-mentioned AKD emulsion standing 30 days, 0.03 part of CPAM, 0.3 part of bentonite, form paper stock after mix homogeneously, and copy formulation by quick kayser method sheet forming apparatus and measure about 60g/m2Handsheet, utilizing liquid infiltration method (GB/T5405 2002) to record handsheet degree of sizing is 85s.
Embodiment 4
Emulsifying agent and the preparation of stabilizer: be scattered in 360 parts of water by 0.2 part of hectorite, 2 parts of NaAsps are scattered in 48 parts of water, are sufficiently mixed by two kinds of liquid, with vinegar acid for adjusting pH most 5.5.Using 13 share cationic starches in 337 parts of water gelatinizing as stabilizer.The two be separately heated to 65 DEG C standby.
The emulsifying of AKD: weigh industrial goods AKD 40 parts, it is heated to 65 DEG C to melt, the emulsifying agent of above-mentioned preparation is added in melted AKD, keeping emulsifying temperature is 65 DEG C, utilize high-speed mixing equipment stirring and emulsifying 15 minutes under 6000 revs/min of rotating speeds, be subsequently added the cationic starch dextrin of 65 DEG C, maintain rotating speed to continue emulsifying 5 minutes, cooling, the AKD emulsion prepared is homogeneous milky oil-in-water type (O/W) emulsion.The mass percent of AKD is about 5%, and emulsion particle diameter is 1~3 μm.
Plasm-glue-blending effect: take 100 parts of hardwood chemical pulps and be dispersed in 9900 parts of water, after being uniformly dispersed, add the 2 parts of above-mentioned AKD emulsions standing 30 days, 0.03 part of CPAM, 0.3 part of bentonite, form paper stock after mix homogeneously, and copy formulation by quick kayser method sheet forming apparatus and measure about 60g/m2Handsheet, utilizing liquid infiltration method (GB/T5405 2002) to record handsheet degree of sizing is 56s.
Embodiment 5
Emulsifying agent and the preparation of stabilizer: be scattered in 399 parts of water by 1 part of hectorite, 0.5 part of NaAsp is scattered in 19.5 parts of water, is sufficiently mixed by two kinds of liquid, is 3.5 with salt acid for adjusting pH value;Using 20 parts of cationic starches in 460 parts of water gelatinizing as stabilizer.The two be separately heated to 65 DEG C standby.
The emulsifying of AKD: weigh industrial goods AKD 100 parts, it is heated to 60 DEG C to melt, the emulsifying agent of above-mentioned preparation is added in melted AKD, keeping emulsifying temperature is 60 DEG C, utilize high-speed mixing equipment stirring and emulsifying 5 minutes under 9000 revs/min of rotating speeds, adding the cationic starch dextrin of 60 DEG C, maintain rotating speed to continue emulsifying 2 minutes, the AKD emulsion prepared is homogeneous milky oil-in-water type (O/W) emulsion.The mass percent of AKD is about 10%, and emulsion particle diameter is 1~3 μm.
Plasm-glue-blending effect: take 50 parts of Straw Pulp and 50 parts of softwood pulps are dispersed in 9900 parts of water, after being uniformly dispersed, add the 1 part of above-mentioned AKD emulsion standing 30 days, 0.03 part of CPAM, 0.3 part of bentonite, form paper stock after mix homogeneously, and copy formulation by quick kayser method sheet forming apparatus and measure about 60g/m2Handsheet, utilizing liquid infiltration method (GB/T5405 2002) to record handsheet degree of sizing is 63s.
Embodiment 6
Emulsifying agent and the preparation of stabilizer: be scattered in 227.5 parts of water by 2.5 parts of hectorites, 1 part of sodium glutamate is scattered in 19 parts of water, is sufficiently mixed by two kinds of liquid, is 4 with salt acid for adjusting pH value;Using 20 parts of cationic starches in 130 parts of water gelatinizing as stabilizer.The two be separately heated to 65 DEG C standby.
The emulsifying of AKD: weigh industrial goods AKD 100 parts, it is heated to 65 DEG C melt, the emulsifying agent of above-mentioned preparation is added in melted AKD, keeping emulsifying temperature is 65 DEG C, utilize high-speed mixing equipment stirring and emulsifying 8 minutes under 10000 revs/min of rotating speeds, being subsequently added the cationic starch dextrin of 65 DEG C, continue emulsifying 4 minutes, the AKD emulsion prepared is homogeneous milky oil-in-water type (O/W) emulsion.The mass percent of AKD is about 20%, and emulsion particle diameter is 1~3 μm.
Plasm-glue-blending effect: take 100 parts of bleaching needle-point leaf pulps and be dispersed in 9900 parts of water, after being uniformly dispersed, add the 0.6 part of above-mentioned AKD emulsion standing 30 days, 0.03 part of CPAM, 0.3 part of bentonite, paper stock is formed after mix homogeneously, and copy formulation by quick kayser method sheet forming apparatus and measure the handsheet of about 60g/m2, utilizing liquid infiltration method (GB/T5405 2002) to record handsheet degree of sizing is 75s.

Claims (8)

1. the preparation method of a surfactant-free alkyl ketene dimer emulsion, it is characterised in that comprise the following steps:
(1) preparation of emulsifying agent aqueous phase: hectorite is used deionized water moistening, dispersion prepare hectorite colloid, uniformly mix with the aqueous solution of water soluble amino acid sodium-salt, be 3~7 with dilute acid for adjusting pH value;
(2) preparation of stabilizer aqueous phase: by cationic starch abundant gelatinizing in water;
(3) prepared by emulsion: melted alkyl ketene dimer, emulsifying agent aqueous phase, stabilizer heated aqueous, by emulsifying agent aqueous phase and melted alkyl ketene dimer liquid mixing, stir under the mechanism of mulser, add stabilizer aqueous phase, continue stirring, obtain emulsion, cooling, obtain stable O/W type alkyl ketene dimer emulsion.
Preparation method the most according to claim 1, it is characterised in that the water soluble amino acid sodium-salt described in step (1) is sodium glutamate or NaAsp.
Preparation method the most according to claim 1, it is characterised in that the diluted acid described in step (1) is one or more in acetic acid, hydrochloric acid, sulphuric acid and citric acid, regulation emulsifying agent aqueous pH values scope is 3.5~5.5.
Preparation method the most according to claim 1, it is characterized in that, hectorite is 1:20~200 with the mass ratio of alkyl ketene dimer, amino acid sodium is 1:20~400 with the mass ratio of alkyl ketene dimer, cationic starch is 1:3~20 with the mass ratio of alkyl ketene dimer, and alkyl ketene dimer is 1:3~19 with aqueous phase total mass ratio in step (1) and (2).
Preparation method the most according to claim 4, it is characterised in that
Hectorite is 1:40~100 with the mass ratio of alkyl ketene dimer;
Amino acid sodium is 1:50~200 with the mass ratio of alkyl ketene dimer;
Cationic starch is 1:4~10 with the mass ratio of alkyl ketene dimer;
Alkyl ketene dimer is 1:4~9 with aqueous phase total mass ratio in step (1) and (2).
Preparation method the most according to claim 1, it is characterised in that in step (3), heating-up temperature is 55~85 DEG C, mulser mixing speed 6000~20000 revs/min, mixing time 2~15 minutes;Continue mixing speed 6000~20000 revs/min, mixing time 2~8 minutes.
Preparation method the most according to claim 6, it is characterised in that in step (3), heating-up temperature is 65~75 DEG C, mulser mixing speed 9000~15000 revs/min, mixing time 3~10 minutes;Continue mixing speed 9000~15000 revs/min, mixing time 3~5 minutes.
8. according to the preparation method one of claim 1-7 Suo Shu, it is characterised in that the cationic starch described in step (2) is the cationic starch that corn starch, tapioca or potato starch modification obtain.
CN201610263090.2A 2016-04-26 2016-04-26 A kind of preparation method of surfactant-free alkyl ketene dimer emulsion Active CN105908567B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610263090.2A CN105908567B (en) 2016-04-26 2016-04-26 A kind of preparation method of surfactant-free alkyl ketene dimer emulsion

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610263090.2A CN105908567B (en) 2016-04-26 2016-04-26 A kind of preparation method of surfactant-free alkyl ketene dimer emulsion

Publications (2)

Publication Number Publication Date
CN105908567A true CN105908567A (en) 2016-08-31
CN105908567B CN105908567B (en) 2017-09-19

Family

ID=56752146

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610263090.2A Active CN105908567B (en) 2016-04-26 2016-04-26 A kind of preparation method of surfactant-free alkyl ketene dimer emulsion

Country Status (1)

Country Link
CN (1) CN105908567B (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107476124A (en) * 2017-09-08 2017-12-15 青岛科技大学 A kind of preparation method of W/O/W types AKD multiple emulsions
CN108425275A (en) * 2018-04-25 2018-08-21 齐鲁工业大学 A kind of preparation method and products thereof of AKD paper sizings agent
CN110004766A (en) * 2019-04-29 2019-07-12 齐鲁工业大学 A kind of alginate coated caco3 particle stablizes the preparation method of paper-making sizing agent emulsion
CN116641256A (en) * 2023-07-10 2023-08-25 上海东升新材料有限公司 Intercalated hydrotalcite stabilized AKD emulsion and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4861376A (en) * 1988-11-10 1989-08-29 Hercules Incorporated High-solids alkyl ketene dimer dispersion
CN101096829A (en) * 2007-07-13 2008-01-02 天津科技大学 Kation alkyl ketene dimer sizing agent and method for making same
CN101736651A (en) * 2009-12-02 2010-06-16 山东轻工业学院 Method for preparing AKD emulsion sizing agent
CN102535248A (en) * 2011-12-30 2012-07-04 广州星业科技股份有限公司 Preparing method for AKD (Alkyl Ketene Dimer) latex

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4861376A (en) * 1988-11-10 1989-08-29 Hercules Incorporated High-solids alkyl ketene dimer dispersion
CN101096829A (en) * 2007-07-13 2008-01-02 天津科技大学 Kation alkyl ketene dimer sizing agent and method for making same
CN101736651A (en) * 2009-12-02 2010-06-16 山东轻工业学院 Method for preparing AKD emulsion sizing agent
CN102535248A (en) * 2011-12-30 2012-07-04 广州星业科技股份有限公司 Preparing method for AKD (Alkyl Ketene Dimer) latex

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
张美云: "《造纸技术》", 31 January 2014, 北京:中国轻工业出版社 *
赵奇: ""改性锂皂石乳化AKD及其乳液的应用研究"", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107476124A (en) * 2017-09-08 2017-12-15 青岛科技大学 A kind of preparation method of W/O/W types AKD multiple emulsions
CN108425275A (en) * 2018-04-25 2018-08-21 齐鲁工业大学 A kind of preparation method and products thereof of AKD paper sizings agent
CN108425275B (en) * 2018-04-25 2020-05-01 齐鲁工业大学 Preparation method of AKD paper sizing agent and product thereof
CN110004766A (en) * 2019-04-29 2019-07-12 齐鲁工业大学 A kind of alginate coated caco3 particle stablizes the preparation method of paper-making sizing agent emulsion
CN110004766B (en) * 2019-04-29 2021-05-18 齐鲁工业大学 Preparation method of alginate-coated calcium carbonate particle stable papermaking sizing agent emulsion
CN116641256A (en) * 2023-07-10 2023-08-25 上海东升新材料有限公司 Intercalated hydrotalcite stabilized AKD emulsion and preparation method thereof

Also Published As

Publication number Publication date
CN105908567B (en) 2017-09-19

Similar Documents

Publication Publication Date Title
US5969011A (en) Sizing of paper
AU729833B2 (en) Sizing of paper
CN105908567A (en) Method for preparing alkyl ketene dimer emulsion without surfactants
US6165259A (en) Aqueous dispersions of hydrophobic material
CN101736651B (en) Method for preparing AKD emulsion sizing agent
CN110004766B (en) Preparation method of alginate-coated calcium carbonate particle stable papermaking sizing agent emulsion
JP4262302B2 (en) Sizing composition
EP1611284A1 (en) Dispersion
EP0961855B1 (en) Aqueous dispersions of a hydrophobic sizing agent
CN102493275A (en) Stable ASA (Alkenyl Succinic Anhydride) papermaking sizing emulsion and preparation method thereof
CN105696417B (en) A kind of preparation method of the AKD emulsions of surfactant-free
US8163133B2 (en) Dispersion
CN101942780B (en) Method for preparing AKD emulsion sizing agent
CN103451995B (en) ASA sizing emulsions that a kind of quaternary ammonium salt-modified hectorite is stable and preparation method thereof
CN103451994B (en) The method of quaternary ammonium salt-modified hectorite emulsifying agent and emulsification ASA thereof a kind of
CN107447580B (en) A kind of emulsifier and a kind of ASA sizing agent emulsion of ASA
CN107489064A (en) A kind of preparation method of the AKD emulsions of activating agent
CN101574834B (en) Method for preparing high-stabliliy ASA papermaking sizing agent emulsion
CN102493276B (en) Stable alkenyl succinic anhydride sizing emulsion for papermaking and preparation method thereof
CN103437244B (en) Melamine modified hectorite stabilized ASA (alkenyl succinic anhydride) sizing emulsion and preparation method thereof
CN113186752A (en) Boron crosslinked organic compound gel emulsifier
CN107447581A (en) A kind of compound emulsifying agent of ASA emulsions and the stabilising system of ASA emulsion sizing agents
CN103451996B (en) A kind of method of cyanurotriamide modified hectorite emulsifying agent and emulsification ASA thereof
WO1998000606A1 (en) Paper sizing composition and process

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
TR01 Transfer of patent right

Effective date of registration: 20200813

Address after: 272100 No. 1, Sun Road, Yanzhou District, Shandong, Jining

Patentee after: SHANDONG XILAI STARCH Co.,Ltd.

Address before: 250399, 3501, University Road, Changqing District, Shandong, Ji'nan

Patentee before: Qilu University of Technology

TR01 Transfer of patent right