CN110485198A - Radiation modification cellulose emulsifier and the AKD lotion prepared using the emulsifier - Google Patents
Radiation modification cellulose emulsifier and the AKD lotion prepared using the emulsifier Download PDFInfo
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- CN110485198A CN110485198A CN201810460609.5A CN201810460609A CN110485198A CN 110485198 A CN110485198 A CN 110485198A CN 201810460609 A CN201810460609 A CN 201810460609A CN 110485198 A CN110485198 A CN 110485198A
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- cellulose
- emulsifier
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
- C08F251/02—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof on to cellulose or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/30—Introducing nitrogen atoms or nitrogen-containing groups
- C08F8/32—Introducing nitrogen atoms or nitrogen-containing groups by reaction with amines
-
- 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
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/03—Non-macromolecular organic compounds
- D21H17/04—Hydrocarbons
-
- 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
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/33—Synthetic macromolecular compounds
- D21H17/34—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D21H17/38—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing crosslinkable groups
- D21H17/39—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing crosslinkable groups forming ether crosslinkages, e.g. alkylol groups
-
- 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
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/63—Inorganic compounds
- D21H17/66—Salts, e.g. alums
-
- 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)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses a kind of radiation modification cellulose emulsifiers; it is to be obtained by epoxychloropropane, triethylamine, radiation modification cellulose, the reaction of first alcohol and water; the radiation modification cellulose is then formed to the surface of cellulose through acetylation and amination using radiation method induction styrene-grafted.The invention also discloses a kind of AKD lotions, including AKD wax and a effective amount of radiation modification cellulose emulsifier.The present invention passes through a series of cellulose modified, a kind of radiation modification cellulose emulsifier is successfully prepared, and obtains a kind of new A KD lotion haveing excellent performance in turn, which has curing speed fast, the high feature of degree of sizing, is with a wide range of applications in field of papermaking.
Description
Technical field
The present invention relates to papermaking AKD sizing agent fields, and in particular to a kind of radiation modification cellulose emulsifier and using should
The AKD lotion of emulsifier preparation.
Background technique
The purpose of sizing is to make Paper or cardboard with the ability of resistance liquid diffusion and infiltration, is suitable for writing and resists with moisture-proof
It is wet.In this course, neutral sizing agent AKD is widely paid close attention to due to its good performance.
AKD is waxy solid, itself does not have charge, therefore can not keep on fiber, is needed using cation emulsified
Agent makes it with positive charge, is adsorbed on fiber and reacts, and generates glue blending function.In early days, general to be formed sediment using cation
Powder is as emulsifier.Since the starch quantity of electric charge is lower, the retention on fiber is low, and easily goes mouldy, to the stabilization of lotion
Property and later period sizing efficiency can have an impact.Cellulose be the most abundant natural polysaccharide material, molecular weight 50,000-250 in the world
Ten thousand.Since its is cheap, and density is low, the process flexibility having had, it is often more important that its hydrophily and extensive chemistry
Modifying Capability is very suitable to prepare natural polymer emulsifier modified AKD emulsion.
Summary of the invention
The object of the present invention is to provide a kind of radiation modification cellulose emulsifiers, and using the radiation modification cellulose cream
The AKD lotion of agent preparation, to solve drawbacks described above existing for background technique.
The present invention realizes by the following technical solutions:
A kind of radiation modification cellulose emulsifier, be by epoxychloropropane, triethylamine, radiation modification cellulose, methanol and
Water reaction obtains, and the radiation modification cellulose is using radiation method induction styrene-grafted to the surface of cellulose, then
It is formed through acetylation and amination.
Following method preparation can be used in the radiation modification cellulose:
Cellulose is immersed in the methanol solution of styrene by step 1, is swollen cellulose sufficiently；
Step 2 utilizes under oxygen-free environment60Co γ pre-irradiation induces styrene-grafted to the surface of cellulose；
The styrene grafted fibre element that upper step obtains is mixed with aluminium chloride, is dispersed in q. s. methylene chloride by step 3
Reaction；
The acetylate that upper step obtains is dispersed in appropriate tetrahydrofuran by step 4, then with diethylamine and carbonic acid
It is sufficiently reacted after the mixing of hydrogen sodium；
Step 5 sufficiently impregnates the aminate that upper step obtains in acid solution, product is washed, it is dry after obtain institute
State radiation modification cellulose.
Preferably, the radiation absorber amount in step 2 is 20-50Gy.
Preferably, the weight ratio of cellulose and styrene is 1:0.8-1.2 in step 1；
Into step 5, the dosage of each component is respectively as follows: step 2 by weight
Preferably, the reaction temperature of step 4 is 65-75 DEG C.
In step 1, the concentration of styrene methanol solution is preferably 3-5mol/L, and soaking time is generally on 24 hours left sides
The right side, so that cellulose is sufficiently swollen.The oxygen-free environment of step 2 can remove oxygen in nitrogen environment repeatedly；Irradiation is anti-
After answering, most handy toluene or other organic solvents wash away unreacted monomer, then drying for standby.In step 3, dichloro
Methane is as reaction dissolvent, and dosage is not particularly limited, and those skilled in the art can be adjusted according to reaction condition；
Acetylate is preferably used to tetrahydrofuran and deionized water washes clean respectively after the reaction was completed, then drying for standby.Step
Four reaction product is preferably washed with distilled water completely, then drying for standby.The acid solution of step 5 can be using 1mol/L's
Hydrochloric acid solution can also use other common acid solutions.
The preferred particle size range of cellulose is at 90-150 μm.
As a preferred technical solution, in the radiation modification cellulose emulsifier, the parts by weight of each component are as follows:
First alcohol and water is as reaction dissolvent, and dosage is not particularly limited, and those skilled in the art can be according to reaction
Condition is adjusted.Preferably, the dosage of methanol is 50-200 parts by weight, and the dosage of water is 50-200 parts by weight.
The preparation method of above-mentioned radiation modification cellulose emulsifier, include the following steps: by epoxychloropropane, triethylamine,
First alcohol and water mixes, and reacts at 40-50 DEG C 2-3 hours, and the radiation modification that then will be scattered in appropriate sodium hydrate aqueous solution is fine
The reaction was continued 2-3 hours in dimension element addition reaction system, obtains the radiation modification cellulose emulsifier.
The concentration and dosage of sodium hydrate aqueous solution are not particularly limited, as long as the fully dispersed radiation modification cellulose of energy is
Can, those skilled in the art can be readily according to the dispersion of radiation modification cellulose to the concentration of sodium hydrate aqueous solution
It is adjusted with dosage.
The present invention further provides the AKD lotions using the preparation of above-mentioned radiation modification cellulose emulsifier, including weigh as follows
Measure the component of part:
100-200 parts of radiation modification cellulose emulsifier,
200-500 parts of AKD wax.
It as a preferred technical solution, can also include the stabilization aid of 3-5 parts by weight in above-mentioned AKD emulsion components.
Preferably, the stabilization aid is selected from High-purity Polyaluminum Chloride, Polyamide-Polyamsne-Epichlorohydrin resin and carbonic acid
The one or more of hydrogen sodium.
The present invention further provides the methods for preparing AKD lotion using radiation modification cellulose emulsifier, including walk as follows
It is rapid: by AKD wax heating melting, to be slowly added to the radiation modification cellulose emulsifier, then high speed shearing emulsification is added and stablizes
Auxiliary agent simultaneously needs to be added a certain amount of water according to solid content, continues high shear agitation, obtains the AKD lotion.
The high speed shear under the revolving speed of 5000-8000r/min as a preferred technical solution,.High speed shearing emulsification when
Between be not particularly limited, can be adjusted according to practical emulsifying effectiveness, usually at 2-3 minutes.
The present invention successfully prepares a kind of radiation modification cellulose emulsifier, and in turn by a series of cellulose modified
A kind of new A KD lotion haveing excellent performance is obtained, which has curing speed fast, the high feature of degree of sizing, leads in papermaking
Domain is with a wide range of applications.
Specific embodiment
The present invention is illustrated below by specific embodiment, but is not intended to limit the present invention.
Embodiment 1:
The present embodiment technical solution is as follows:
1. being impregnated firstly, being 3mol/L by the concentration that cellulose is immersed in styrene in the mixed liquor of styrene and methanol
24 hours, so that cellulose is sufficiently swollen, then in nitrogen environment, oxygen is removed repeatedly.It utilizes60The induction of Co γ pre-irradiation
The table absorbed dose of styrene-grafted to cellulose is 20Gy, washes away unreacted monomer with toluene, and dry 24 is small at 50 DEG C
When.Then, it by 100 parts of above-mentioned products and 120g parts of aluminium chloride, is dispersed in suitable methylene chloride, reacts under agitation
7 hours, then product is used to tetrahydrofuran and deionized water washes clean respectively, it is 24 hours dry at 50 DEG C.By above-mentioned production
Object is added in appropriate tetrahydrofuran, and 300 parts of diethylamine and 30 parts of sodium bicarbonates are added, and reacts 2 hours at 70 DEG C, so
Product is washed with distilled water completely afterwards, 24 hours dry at 50 DEG C.It is impregnated in the hydrochloric acid of 1mol/L finally, product will be obtained
24 hours, product was washed with distilled water completely, 24 hours dry at 50 DEG C.
2. by mass, by 80 parts of epoxychloropropane, 100 parts of methanol, 100 parts of water, 100 parts of triethylamines are uniformly mixed, and 45
It is reacted 2 hours at DEG C.
3. after being dissolved in NaOH solution, being added in above-mentioned system then by 100 parts of radiation modification cellulose, continue
Reaction 2 hours, obtains a kind of radiation modification cellulose emulsifier.
4. 200 parts of AKD wax water-baths are melted, above-mentioned radiation modification cellulose emulsifier solution is slowly added to, 5000r/
Min emulsification pretreatment 3 minutes, 3 parts of High-purity Polyaluminum Chlorides are added, it is quick after five minutes to continue high shear agitation for 200 parts of water
Cooling, discharging.
Embodiment 2
The present embodiment technical solution is as follows:
1. being impregnated firstly, being 5mol/L by the concentration that cellulose is immersed in styrene in the mixed liquor of styrene and methanol
24 hours, so that cellulose is sufficiently swollen, then in nitrogen environment, oxygen is removed repeatedly.It utilizes60The induction of Co γ pre-irradiation
The table absorbed dose of styrene-grafted to cellulose is 50Gy, washes away unreacted monomer with toluene, and dry 24 is small at 50 DEG C
When.Then, it by 100 parts of above-mentioned products and 1150g parts of aluminium chloride, is dispersed in suitable methylene chloride, under agitation instead
It answers 7 hours, then product is used to tetrahydrofuran and deionized water washes clean respectively, it is 24 hours dry at 50 DEG C.It will be above-mentioned
Product is added in appropriate tetrahydrofuran, and 400 parts of diethylamine and 30 parts of sodium bicarbonates are added, and is reacted 2 hours at 70 DEG C,
Then product is washed with distilled water completely, 24 hours dry at 50 DEG C.It is soaked in the hydrochloric acid of 1mol/L finally, product will be obtained
Bubble 24 hours, product is washed with distilled water completely, 24 hours dry at 50 DEG C.
2. by mass, by 800 parts of epoxychloropropane, 100 parts of methanol, 100 parts of water, 120 parts of triethylamines are uniformly mixed, and 40
It is reacted 3 hours at DEG C.
3. after being dissolved in NaOH solution, being added in above-mentioned system then by 100 parts of radiation modification cellulose, continue
Reaction 3 hours, obtains a kind of radiation modification cellulose emulsifier.
4. 500 parts of AKD wax water-baths are melted, above-mentioned radiation modification cellulose emulsifier solution is slowly added to, 8000r/
Min emulsification pretreatment 3 minutes, 5 parts of Polyamide-Polyamsne-Epichlorohydrin resins are added, 500 parts of water continues high shear agitation 10
It is quickly cooled down after minute, discharging.
Embodiment 3
The present embodiment technical solution is as follows:
1. the concentration of styrene is 3mol/L firstly, cellulose is immersed in the mixed liquor of styrene and methanol, impregnate
24 hours, so that cellulose is sufficiently swollen, then in nitrogen environment, oxygen is removed repeatedly.It utilizes60The induction of Co γ pre-irradiation
The table absorbed dose of styrene-grafted to cellulose is 40Gy, washes away unreacted monomer with toluene, and dry 24 is small at 50 DEG C
When.Then, it by 100 parts of above-mentioned products and 130g parts of aluminium chloride, is dispersed in suitable methylene chloride, reacts under agitation
7 hours, then product is used to tetrahydrofuran and deionized water washes clean respectively, it is 24 hours dry at 50 DEG C.By above-mentioned production
Object is added in appropriate tetrahydrofuran, and 350 parts of diethylamine and 50 parts of sodium bicarbonates are added, and reacts 2 hours at 70 DEG C, so
Product is washed with distilled water completely afterwards, 24 hours dry at 50 DEG C.It is impregnated in the hydrochloric acid of 1mol/L finally, product will be obtained
24 hours, product was washed with distilled water completely, 24 hours dry at 50 DEG C.
2. by mass, by 90 parts of epoxychloropropane, 100 parts of methanol, 100 parts of water, 110 parts of triethylamines are uniformly mixed, and 40
It is reacted 2 hours at DEG C.
3. after being dissolved in NaOH solution, being added in above-mentioned system then by 100 parts of radiation modification cellulose, continue
Reaction 3 hours, obtains a kind of radiation modification cellulose emulsifier.
4. 400 parts of AKD wax water-baths are melted, above-mentioned radiation modification cellulose emulsifier solution is slowly added to, 7000r/
Min emulsification pretreatment 2 minutes, 3 parts of sodium bicarbonates are added, 400 parts of water is quickly cooled down after continuing high shear agitation 8 minutes, goes out
Material.
Embodiment 4
The present embodiment technical solution is as follows:
1. being impregnated firstly, being 4mol/L by the concentration that cellulose is immersed in styrene in the mixed liquor of styrene and methanol
24 hours, so that cellulose is sufficiently swollen, then in nitrogen environment, oxygen is removed repeatedly.It utilizes60The induction of Co γ pre-irradiation
The table absorbed dose of styrene-grafted to cellulose is 35Gy, washes away unreacted monomer with toluene, and dry 24 is small at 50 DEG C
When.Then, it by 100 parts of above-mentioned products and 150g parts of aluminium chloride, is dispersed in suitable methylene chloride, reacts under agitation
7 hours, then product is used to tetrahydrofuran and deionized water washes clean respectively, it is 24 hours dry at 50 DEG C.By above-mentioned production
Object is added in appropriate tetrahydrofuran, and 350 parts of diethylamine and 30 parts of sodium bicarbonates are added, and reacts 2 hours at 70 DEG C, so
Product is washed with distilled water completely afterwards, 24 hours dry at 50 DEG C.It is impregnated in the hydrochloric acid of 1mol/L finally, product will be obtained
24 hours, product was washed with distilled water completely, 24 hours dry at 50 DEG C.
2. by mass, by 100 parts of epoxychloropropane, 100 parts of methanol, 100 parts of water, 120 parts of triethylamines are uniformly mixed, and 45
It is reacted 3 hours at DEG C.
3. after being dissolved in NaOH solution, being added in above-mentioned system then by 100 parts of radiation modification cellulose, continue
Reaction 2.5 hours, obtains a kind of radiation modification cellulose emulsifier.
4. 370 parts of AKD wax water-baths are melted, above-mentioned radiation modification cellulose emulsifier solution is slowly added to, 6500r/
Min emulsification pretreatment 33 minutes, be added 4 parts of sodium bicarbonates, 400 parts of water, continue high shear agitation be quickly cooled down after ten minutes,
Discharging.
Comparative example
Using gelatinized starch AKD lotion as comparative example.
Copy paper:
Selecting mass fraction is 0.5% softwood pulp, and sequence is added the AKD's and 0.02% of oven dry stock quality 0.2%
Cationic polyacrylamide stirs 1min, is eventually adding 20%GCC (grinding calcium carbonate) copy paper after mixing evenly, manufactures paper with pulp quantitative
For 60gm-2Left and right, then after squeezing 1min under 0.4MPa pressure with hydraulic press, (92 DEG C or so) are dried with vacuum drier
4min.Lower machine surveys degree of sizing.Degree of sizing is measured by GB/T5405-1985.
In addition, curing rate calculates according to the following formula:
Measurement result is shown in Table 1.
1 product performance index of table
| Degree of sizing (%) | Curing rate (%) | |
| Comparative example | 51 | 59 |
| Embodiment one | 74 | 81 |
| Embodiment two | 67 | 78 |
| Embodiment three | 67 | 72 |
| Example IV | 69 | 77 |
As can be seen from the results in the table that AKD lotion prepared by the present invention has higher degree of sizing and curing rate.
The above shows and describes the basic principle, main features and advantages of the invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (10)
1. a kind of radiation modification cellulose emulsifier, which is characterized in that be by epoxychloropropane, triethylamine, radiation modification fiber
Element, the reaction of first alcohol and water obtain, and the radiation modification cellulose induces styrene-grafted to cellulose using radiation method
Then surface is formed through acetylation and amination.
2. radiation modification cellulose emulsifier as described in claim 1, which is characterized in that the system of the radiation modification cellulose
Preparation Method includes the following steps:
Cellulose is immersed in the methanol solution of styrene by step 1, is swollen cellulose sufficiently；
Step 2 utilizes under oxygen-free environment60Co γ pre-irradiation induces styrene-grafted to the surface of cellulose；
The styrene grafted fibre element that upper step obtains is mixed with aluminium chloride, is dispersed in q. s. methylene chloride and reacts by step 3；
The acetylate that upper step obtains is dispersed in appropriate tetrahydrofuran by step 4, then with diethylamine and sodium bicarbonate
It is sufficiently reacted after mixing；
Step 5 sufficiently impregnates the aminate that upper step obtains in acid solution, product is washed, it is dry after obtain the spoke
Penetrate modified cellulose.
3. radiation modification cellulose emulsifier as claimed in claim 2, which is characterized in that cellulose and styrene in step 1
Weight ratio be 1:0.8-1.2；Into step 5, the dosage of each component is respectively as follows: step 2 by weight
4. radiation modification cellulose emulsifier as claimed in claim 2, which is characterized in that the radiation absorber amount in step 2
For 20-50Gy, the reaction temperature of step 4 is 65-75 DEG C.
5. radiation modification cellulose emulsifier as claimed in claim 2, which is characterized in that the partial size of the cellulose is 90-
150μm。
6. radiation modification cellulose emulsifier as described in claim 1, which is characterized in that the parts by weight of each component are as follows:
7. the method for preparing the radiation modification cellulose emulsifier as described in claim any one of 1-6, which is characterized in that including such as
Lower step: epoxychloropropane, triethylamine, first alcohol and water being mixed, reacted 2-3 hours at 40-50 DEG C, then will be scattered in appropriate
The reaction was continued 2-3 hours in the radiation modification cellulose addition reaction system of sodium hydrate aqueous solution, obtains the radiation modification
Cellulose emulsifier.
8. a kind of AKD lotion, which is characterized in that including AKD wax and a effective amount of radiation as claimed in any one of claims 1 to 6
Modified cellulose emulsifier.
9. AKD lotion as claimed in claim 8, which is characterized in that the parts by weight of each component are as follows:
100-200 parts of radiation modification cellulose emulsifier,
200-500 parts of AKD wax.
10. AKD lotion as claimed in claim 9, which is characterized in that further include the stabilization aid of 3-5 parts by weight, the stabilization
Auxiliary agent is selected from the one or more of High-purity Polyaluminum Chloride, Polyamide-Polyamsne-Epichlorohydrin resin and sodium bicarbonate.
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| WO2000034583A1 (en) * | 1998-12-07 | 2000-06-15 | Hercules Incorporated | Sizing composition |
| CN1715552A (en) * | 2004-06-30 | 2006-01-04 | 桂林正翰科技开发有限责任公司 | Novel method for preparing ion exchange fiber by graft copolymerization |
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