CN106087561A - A kind of paper strengthening agent and production method thereof - Google Patents

A kind of paper strengthening agent and production method thereof Download PDF

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Publication number
CN106087561A
CN106087561A CN201610411295.0A CN201610411295A CN106087561A CN 106087561 A CN106087561 A CN 106087561A CN 201610411295 A CN201610411295 A CN 201610411295A CN 106087561 A CN106087561 A CN 106087561A
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China
Prior art keywords
paper
temperature
minutes
paper pulp
pulp fiber
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CN201610411295.0A
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Chinese (zh)
Inventor
宋先亮
闫琳雨
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Beijing Forestry University
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Beijing Forestry University
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Priority to CN201610411295.0A priority Critical patent/CN106087561A/en
Publication of CN106087561A publication Critical patent/CN106087561A/en
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    • 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
    • D21H21/18Reinforcing agents

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Abstract

A kind of paper strengthening agent and production method thereof, be configured to mixture aqueous solution with the trimesic acid of paper pulp fiber absolute dry mass 4%~13% and the sodium dihydric hypophosphite of 2%~7%;Paper pulp fiber is added in described mixture aqueous solution, is configured to the slurry that pulp content is 1wt% ~ 3wt%, process 110~130 minutes at a temperature of 20~30 DEG C;It is warming up to 75~90 DEG C, processes 20~40 minutes at such a temperature;It is continuously heating to 150~170 DEG C, processes 20~40 minutes at such a temperature;Products therefrom temperature be 20~30 DEG C water washing after filter prepare.Use sodium dihydric hypophosphite can improve reaction efficiency as catalyst, reduce reaction temperature;In paper pulp, small short fibers is as raw material, it is achieved the comprehensive utilization of fibre resources.

Description

A kind of paper strengthening agent and production method thereof
Technical field
The present invention relates to the paper strengthening agent of paper technology, particularly to a kind of paper strengthening agent and production method thereof.
Background technology
Along with China's expanding economy and the raising of people's living standard, the demand of paper is constantly increased by people, right The requirement of paper quality is more and more higher, has largely promoted the development of China's paper industry.But China's paper industry raw material Present situation is: timber resources is rare, and log slurry proportion is less;Straw Pulp and reclaimed waste paper slurry proportion are more.And wheat straw The a large amount of use of slurry and recovery slurry will certainly affect paper quality, reduces paper performance.Strengthening for paper is added in paper-making process Agent can be effectively improved this situation, can be effectively improved Straw Pulp and secondary stock paper properties, improves paper quality, expands useless The range of paper pulp.
CN103726379A discloses the application as paper making intensifier of a kind of modified Nano microcrystalline Cellulose.To bleach pin Leaf wood sulfate pulp, bleaching broad-leaved wood sulphate pulp, microcrystalline Cellulose or Cotton Gossypii are raw material, use following acid-hydrolysis method or biology Enzyme hydrolysis method prepares nano micro crystal cellulose: acid-hydrolysis method: by raw material pulverizing, crosses 20 mesh sieves, adds 30-under 20 C-65 C The sulphuric acid of 64wt%, makes acid and the volume mass ratio (5~15) of raw material: 1, and unit milliliter Bick, raw material is in terms of over dry material;Stirring Under, react 10min-70min, then dilute to terminate reaction, products therefrom by the suspension deionized water of 9-10 times of volume It is centrifuged repeatedly with deionized water and rinses to pH value 5.0~5.5, product will be obtained and put in bag filter, with the deionized water of flowing Dialysing constant to pH value, the suspension after dialysis carries out supersonic oscillations in ice-water bath and processes 5min-50min, obtains nanometer Microcrystal cellulose colloid suspension;Or, biological enzyme hydrolysis method: by raw material pulverizing, cross 20 mesh sieves, raw material is put in conical flask, Adding water in conical flask, the pH value adding buffer regulation solution adds to 6-7, addition cellulase, every gram of over dry raw material Cellulase 5000~80000IU, is placed in shaking table, and regulation temperature is 40 C~60 C, hunting speed 50~250r/min, instead Answer 24h-72h, after reaction terminates, add ethanol enzymolysis reaction, take out sample, be centrifuged repeatedly washing with deionized water, wash Suspension ultrasonic oscillator after washing processes 5min~50min, obtains Nanocrystalline Cellulose Colloid suspension;Described fibre Dimension element enzyme is the neutral cellulase that jade of the He family Bioisystech Co., Ltd produces, its filter paper enzyme activity 20000~40000IU/g, Described buffer is phosphate buffered solution, takes sodium dihydrogen phosphate 1.74g, disodium hydrogen phosphate 2.7g, sodium chloride 1.7g, adds water-soluble Solution becomes the solution of 400ml formulated;(2) modification of nano micro crystal cellulose is carried out as follows: take 1g(over dry) step (1) the nano micro crystal cellulose suspension prepared, is sequentially added into 3.0~8.0mmolNaBr, 0.005~0.03mmol2, and 2,6, 6-tetramethyl-1-piperidines oxygen and the NaClO solution of 1~15mmol, add the Na of 200ml~250ml pH=10.22CO3- NaHCO3Buffer solution, regulation system pH to 10~10.5, then carry out ultrasonic disperse (ultrasonic 1s, 8s gap) 5min~ 20min, reacts 10min~60min at 25 C~60 C, adds 10ml~20ml dehydrated alcohol and terminates reaction, adjusts pH to 7 with acid Left and right, dialyses 2~5 days, obtains modified Nano microcrystalline Cellulose suspension, be reinforcing agent;Or, take 1g(over dry) and step (1) prepare nano micro crystal cellulose suspension, add 0.2M acetate buffer solution 200~300ml, be separately added into 5~ 20mmol/gNaClO2And 0.2~0.5mmol/g4-acetylaminohydroxyphenylarsonic acid 2,2,6,6-tetramethyl-1-piperidines oxygen, be subsequently adding 1~ The NaClO solution of 5mmol/g, regulation pH value to 4.8, under 30 C~80 C stirring reaction 2~5 days, be subsequently adding 10~ 20ml dehydrated alcohol terminates reaction, dialyses 2~5 days, obtains modified Nano microcrystalline Cellulose suspension, be reinforcing agent.
Nano micro crystal cellulose preparation process in above-mentioned patent is complicated, and the pollution utilizing acid hydrolysis process to produce is big, profit With cellulose degraded time length, cost height, follow-up 2,2,6,6-tetramethyl-1-piperidines oxygen are the method for modifying cost of medium High, it is difficult to industrialization.
Summary of the invention
In order to overcome the deficiencies in the prior art, it is an object of the invention to provide a kind of paper strengthening agent and producer thereof Method.
In order to solve above-mentioned technical problem, on the one hand, a kind of paper strengthening agent that the present invention provides, by following methods system : it is configured to mixture water with the trimesic acid of paper pulp fiber absolute dry mass 4%~13% and the sodium dihydric hypophosphite of 2%~7% Solution;Paper pulp fiber is added in described mixture aqueous solution, is configured to the slurry that pulp content is 1wt% ~ 3wt%, this slurry Process 110~130 minutes at a temperature of 20~30 DEG C;It is warming up to 75~90 DEG C, processes 20~40 minutes at such a temperature;Continue It is warming up to 150~170 DEG C, processes 20~40 minutes at such a temperature;After products therefrom temperature is the water washing of 20~30 DEG C Filter.
As improving technical scheme further, the paper strengthening agent that the present invention provides, described paper pulp fiber is below 100 mesh Short and small paper pulp fiber.
As improving technical scheme further, the paper strengthening agent that the present invention provides, described mixture aqueous solution is paper using The mixture aqueous solution that the trimesic acid of pulp fibres absolute dry mass 7%~13% and the sodium dihydric hypophosphite of 3%~7% are configured to.
In order to solve above-mentioned technical problem, on the other hand, the production method of a kind of paper strengthening agent that the present invention provides, bag Include following steps: be configured to the trimesic acid of paper pulp fiber absolute dry mass 4%~13% and the sodium dihydric hypophosphite of 2%~7% Mixture aqueous solution;Paper pulp fiber is added in described mixture aqueous solution, is configured to the slurry that pulp content is 1wt% ~ 3wt% Material, this slurry processes 110~130 minutes at a temperature of 20~30 DEG C;It is warming up to 75~90 DEG C, processes 20~40 at such a temperature Minute;It is continuously heating to 150~170 DEG C, processes 20~40 minutes at such a temperature;Products therefrom temperature is 20~30 DEG C Filter after water washing.
As improving technical scheme further, the production method of the paper strengthening agent that the present invention provides, described paper pulp fiber It it is the short and small paper pulp fiber of below 100 mesh.
As improving technical scheme further, the production method of the paper strengthening agent that the present invention provides, described mixture water Solution is the mixing that is configured to of sodium dihydric hypophosphite of the trimesic acid with paper pulp fiber absolute dry mass 7%~13% and 3%~7% Thing aqueous solution.
The beneficial effect that the present invention brings: use sodium dihydric hypophosphite reaction efficiency can be greatly improved as catalyst, fall Low reaction temperatures.Trimesic acid makes reaction with the hydroxyl reaction in fiber under conditions of reaction temperature and catalyst exist Connect the compound containing many carboxyls on product fibrous strands, increase the carboxyl-content on fiber.When paper strengthening agent adds paper pulp to In when manufacturing paper with pulp, the adhesion between paper pulp fiber can be strengthened, thus improve the physical strength of paper.With small short fibers in paper pulp it is Raw material, it is achieved the comprehensive utilization of fiber fines resource.
The present invention may utilize the small short fibers that pulp beating obtains can prepare height through trimesic acid esterification treatment The paper strengthening agent of performance, raw material is easy to get, preparation process simple, reaction condition is easily achieved, it is the lowest to pollute, and is suitable for industry Change.
With mixing that the trimesic acid of paper pulp fiber absolute dry mass 7%~13% and the sodium dihydric hypophosphite of 3%~7% are configured to Compound aqueous solution.
Detailed description of the invention
Embodiment 1: by the small short fibers below prepared 100 mesh that sieve after pulp beating;With described paper pulp small short fibers The trimesic acid of 4wt% and the sodium dihydric hypophosphite of 2wt% make aqueous solution;Paper pulp fiber is added described mixture aqueous solution In, it being configured to the slurry that pulp content is 1wt%, this slurry processes 130 minutes at a temperature of 20 DEG C;Rise high-temperature to 75 DEG C, Small short fibers continues with 20 minutes at this temperature;System temperature is increased to 150 DEG C again process 20 minutes.By products therefrom Processing 20 minutes with 20 DEG C of distilled water, filtration drying prepares paper strengthening agent, and carboxyl-content is 56.67mmol/Kg.
Embodiment 2: by the small short fibers below prepared 100 mesh that sieve after pulp beating;With described paper pulp small short fibers The trimesic acid of 7wt% and the sodium dihydric hypophosphite of 3wt% make aqueous solution;Paper pulp fiber is added described mixture aqueous solution In, it being configured to the slurry that pulp content is 1.5wt%, this slurry processes 120 minutes at a temperature of 25 DEG C;Rise high-temperature to 80 DEG C, Small short fibers continues with 30 minutes at this temperature;System temperature is increased to 160 DEG C again process 30 minutes.By products therefrom Processing 30 minutes with 25 DEG C of distilled water, filtration drying prepares paper strengthening agent, and carboxyl-content is 73.33mmol/Kg.
Embodiment 3: by the small short fibers below prepared 100 mesh that sieve after pulp beating;With described paper pulp small short fibers The trimesic acid of 10wt% and the sodium dihydric hypophosphite of 4.5wt% make aqueous solution;Paper pulp fiber is added described mixture water In solution, being configured to the slurry that pulp content is 2wt%, this slurry processes 125 minutes at a temperature of 27 DEG C;Rise high-temperature to 85 DEG C, small short fibers continues with 35 minutes at this temperature;System temperature is increased to 165 DEG C again process 35 minutes.By gained Product processes 35 minutes with 27 DEG C of distilled water, and filtration drying prepares paper strengthening agent, and carboxyl-content is 83.33mmol/Kg.
Embodiment 4: by the small short fibers below prepared 100 mesh that sieve after pulp beating;With described paper pulp small short fibers The trimesic acid of 13wt% and the sodium dihydric hypophosphite of 7wt% make aqueous solution;Paper pulp fiber is added described mixture water-soluble In liquid, being configured to the slurry that pulp content is 3wt%, this slurry processes 110 minutes at a temperature of 30 DEG C;Rise high-temperature to 90 DEG C, Small short fibers continues with 40 minutes at this temperature;System temperature is increased to 170 DEG C again process 40 minutes.By products therefrom Processing 40 minutes with 30 DEG C of distilled water, filtration drying prepares paper strengthening agent, and carboxyl-content is 100mmol/Kg.
In the present invention, the detection of carboxyl-content uses conductance method to measure, particular reference (Katz, S., Beatson, R.P. and Scallan, A.M. Strong and Weak Acidic Groups in Sulfite Pulps, Svensk Papperstidning, 1984 (6): R48~R53) test.
40 are pulled an oar after being discongested by popular Kraft pulp wateroSR, is diluted to the concentration of 2 ‰, adds absolute dried paper pulp 1wt% Embodiment 1 ~ 4 prepares paper strengthening agent, adds the aluminum sulfate of absolute dried paper pulp 0.5wt%, and the pH value of regulation slurry, to 5, stirs After, copy by preparation routine sheet forming apparatus method (QB/T3703-99) of paper pulp laboratory page and take quantitative 60g/m2Page.? At 105 DEG C after ripening 20min, equilibrium water conten 24h under the conditions of constant temperature and humidity, is drawn by the mensuration constant speed of paper and cardboard tensile strength Stretch the mensuration (GB/T 455-2002) of method (100mm/min) (GB/T 22898-2008), paper and cardboard tearability, paper bursting strength Mensuration (GB/T 457-2008) method of mensuration (GB/T 454-2002), paper and cardboard folding strength test.
Reference examples: starch and experimental condition for identical poplar, in the situation being added without the paper strengthening agent that the present invention provides Under trial-production sheet paper products.
Test result such as following table:
Result shows: the increase of the carboxyl-content of the paper strengthening agent obtained along with paper pulp small short fibers modified product, paper Dry tensile strength is in downward trend after first rising;Burst index and dry tensile strength similar trend;Tear index is the most notable to be risen After have bigger decline;Folding strength is slightly downward trend after notable rising in elder generation, but all good than the performance of reference examples, the short and small fibre of paper pulp After dimension carboxyl increases, making the adhesion between fiber increase, tensile index, folding strength increase the most therewith with bursting strength.Preferably Add the trimesic acid of paper pulp small short fibers oven-dry weight 9%~12%, the paper strengthening agent of the secondary diphosphate sodium of 4%~5%, its carboxylic Base content 75~85 mmol/kg, has preferable technique effect.
It is clear that the invention is not restricted to above preferred implementation, also can limit in the claims in the present invention and description In spirit, carry out conversion and the improvement of various ways, same technical problem can be solved, and obtain intended technique effect, therefore Do not repeat.Those of ordinary skill in the art can from present disclosure directly or all schemes of associating, if Within the spirit that claim limits, fall within protection scope of the present invention.

Claims (6)

1. a paper strengthening agent, it is characterised in that prepared by following methods: use the equal of paper pulp fiber absolute dry mass 4%~13% Benzenetricarboxylic acid and 2%~7% sodium dihydric hypophosphite be configured to mixture aqueous solution;Paper pulp fiber is added described mixture water-soluble In liquid, being configured to the slurry that pulp content is 1wt% ~ 3wt%, this slurry processes 110~130 minutes at a temperature of 20~30 DEG C; It is warming up to 75~90 DEG C, processes 20~40 minutes at such a temperature;It is continuously heating to 150~170 DEG C, processes 20 at such a temperature ~40 minutes;Products therefrom temperature be 20~30 DEG C water washing after filter.
Paper strengthening agent the most according to claim 1, it is characterised in that described paper pulp fiber is the short and small of below 100 mesh Paper pulp fiber.
3. the paper strengthening agent described in claim 1 or 2, it is characterised in that described mixture aqueous solution is exhausted with paper pulp fiber The mixture aqueous solution that the trimesic acid of dry mass 7%~13% and the sodium dihydric hypophosphite of 3%~7% are configured to.
4. the production method preparing paper strengthening agent described in claim 1, it is characterised in that comprise the following steps: paper using The trimesic acid of pulp fibres absolute dry mass 4%~13% and the sodium dihydric hypophosphite of 2%~7% are configured to mixture aqueous solution;Will Paper pulp fiber adds in described mixture aqueous solution, is configured to the slurry that pulp content is 1wt% ~ 3wt%, and this slurry is 20~30 Process 110~130 minutes at a temperature of DEG C;It is warming up to 75~90 DEG C, processes 20~40 minutes at such a temperature;It is continuously heating to 150~170 DEG C, process 20~40 minutes at such a temperature;Products therefrom temperature be 20~30 DEG C water washing after filter.
The production method of paper strengthening agent the most according to claim 4, it is characterised in that described paper pulp fiber is 100 mesh Following short and small paper pulp fiber.
The production method of paper strengthening agent the most according to claim 4, it is characterised in that described mixture aqueous solution is for using The mixture that the trimesic acid of paper pulp fiber absolute dry mass 7%~13% and the sodium dihydric hypophosphite of 3%~7% are configured to is water-soluble Liquid.
CN201610411295.0A 2016-06-13 2016-06-13 A kind of paper strengthening agent and production method thereof Pending CN106087561A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000039389A1 (en) * 1998-12-29 2000-07-06 Weyerhaeuser Company Carboxylated cellulosic fibers
CN102852035A (en) * 2012-08-27 2013-01-02 北京林业大学 Paper reinforcing agent, and production and usage method thereof
CN103437246A (en) * 2013-08-30 2013-12-11 华南理工大学 Paper strengthening agent, and preparation method and application thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000039389A1 (en) * 1998-12-29 2000-07-06 Weyerhaeuser Company Carboxylated cellulosic fibers
CN102852035A (en) * 2012-08-27 2013-01-02 北京林业大学 Paper reinforcing agent, and production and usage method thereof
CN103437246A (en) * 2013-08-30 2013-12-11 华南理工大学 Paper strengthening agent, and preparation method and application thereof

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Application publication date: 20161109