CN114263065B - Interlayer reinforcing agent for papermaking, raw material composition thereof and preparation method thereof - Google Patents
Interlayer reinforcing agent for papermaking, raw material composition thereof and preparation method thereof Download PDFInfo
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Abstract
The invention provides an interlaminar reinforcing agent for papermaking, which comprises 100 parts of dissolving pulp prehydrolysis liquid, 10-20 parts of starch, 5-10 parts of acrylamide, 0.5-1 part of acid catalyst, 1-2 parts of inorganic base, 2-4 parts of dialdehyde, 0.5-2 parts of initiator, 1-2 parts of stabilizer and 0.1-0.2 part of complexing agent. The preparation method comprises the steps of adding starch and a complexing agent into dissolving pulp prehydrolysis liquid, heating, adding an acid catalyst, dropwise adding a mixture of dialdehyde and water, keeping the temperature for reaction at the temperature after dropwise adding is finished, then continuously adding inorganic base, dropwise adding an initiator and acrylamide at the same time, keeping the temperature for reaction after dropwise adding is finished, then adding a stabilizer, and cooling to room temperature to prepare the interlayer reinforcing agent for papermaking. The interlaminar reinforcing agent for papermaking takes pulping waste liquid with wide renewable sources as a main raw material, the raw material formula is relatively simple, the preparation steps are simple and easy to operate, and the interlaminar reinforcing agent used for spraying paper can effectively improve the internal combination between fibers and the ring crush value of a paper sample.
Description
Technical Field
The invention relates to the technical field of papermaking reinforcing agents, and particularly relates to an interlayer reinforcing agent for papermaking, a raw material composition of the interlayer reinforcing agent and a preparation method of the interlayer reinforcing agent.
Background
In recent years, sulfate-based dissolving pulp pulping processes have incorporated the concept of biomass refining, with pretreatment to remove hemicellulose prior to pulping to obtain higher quality dissolving pulp. The prehydrolysis liquid contains hemicellulose degradation products, micromolecular lignin, furfural, acetic acid and other products, and the components are recycled, so that the environmental pollution load can be reduced on one hand, and extra economic benefits can be brought to pulping and papermaking enterprises on the other hand.
With the gradual decrease of the total amount of non-renewable resources such as petroleum, coal and the like, the conversion of agricultural and forestry waste renewable resources to obtain new materials, high-calorific-value energy sources, chemical raw materials and medicines is becoming an important development trend, and the modification of natural polymers becomes an important branch in the research and utilization of agricultural and forestry waste renewable resources. Although natural polymers are widely distributed in plants, further modification is required to be utilized because the complexity of the structure limits their use in industry.
In addition, the influence of the prohibition of solid waste import in recent two years makes the fiber raw materials of paper-making enterprises which take waste paper as raw materials worse and worse; meanwhile, as more and more paper making sludge and sawdust manufacturers are added, the quality of white water is poorer and poorer, so that the strength indexes such as the bonding strength between paper layers, the ring crush strength, the bursting strength and the like are reduced, and therefore, a large amount of reinforcing agents are required to be added to compensate the strength of the paper.
In the past, people often use interlayer spraying starch as an interlayer reinforcing agent, but the starch serving as an edible food product of people should meet the national needs firstly. In addition, a number of starch grafted monomers are disclosed as reinforcing agents in general patents, for example, CN111172808A discloses a reinforcing agent for spraying between paper layers and a preparation method thereof, wherein a starch grafted polyacrylamide intermediate is prepared, then polyvinyl alcohol, urea, starch grafted polyacrylamide and dialdehyde are reacted to prepare a dialdehyde modified polyvinyl alcohol-urea-starch grafted polyacrylamide composition with the solid content of 20-40%, the composition is added into a starch dispersion liquid, then a cross-linking agent is added, and the mixture is uniformly stirred to obtain the reinforcing agent for spraying between paper layers. The reinforcing agent is sprayed between paper layers, and after squeezing and drying, the indexes of interlayer bonding strength, ring crush strength, bursting strength, wet strength and the like of the multi-layer composite paper can be obviously improved, so that the reinforcing agent can be widely applied to multi-layer composite paper such as bobbin paper, boxboard paper, white board paper and the like. However, these monomers and the chemicals involved therein are not green, toxic to the human body and high in cost.
The applicant's prior application CN113089368A discloses a natural polymer modified reinforcing agent for spraying between paper layers, which comprises the following components in parts by weight: the paper interlayer spraying reinforcing agent comprises, by weight, 1 part of polysaccharide mixture, 0.03-0.2 part of enzyme preparation or acid, 0.015-0.2 part of cross-linking agent, 0.5-1 part of starch, 0.03-0.6 part of dispersing agent and 1.5-5 parts of water.
At present, no report exists for an interlaminar reinforcing agent for papermaking, which takes dissolving pulp pulping waste liquid as a main raw material.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a nontoxic and harmless reinforcing agent prepared by using the dissolving pulp pulping waste liquid without separation and purification, and the reinforcing agent can be compared with the starch reinforcing agent on the market in performance.
The invention is realized by adopting the following technical scheme:
the invention provides a raw material composition of an interlayer reinforcing agent for papermaking, which comprises the following components in parts by weight: 100 parts of dissolving pulp prehydrolysis liquid, 10-20 parts of starch, 5-10 parts of acrylamide, 0.5-1 part of acid catalyst, 1-2 parts of inorganic base, 2-4 parts of dialdehyde, 0.5-2 parts of initiator, 1-2 parts of stabilizer and 0.1-0.2 part of complexing agent.
The dissolving pulp prehydrolysis liquid is a byproduct for preparing dissolving pulp by adopting a prehydrolysis sulfate method, and the main purpose of the pretreatment process of the dissolving pulp is to hydrolyze and dissolve hemicellulose as much as possible so as to reduce the content of the hemicellulose in the raw material and improve the uniformity of the dissolving pulp. The hydrolysis reaction mechanism of the hemicellulose in the dilute acid pretreatment is H generated by the dissociation of acid in water + Combined with water to produce H 3 O + Which can enableThe O of the glycosidic bond in the hemicellulose macromolecule is quickly protonated to form a conjugate acid, thereby weakening the energy of the glycosidic bond to generate the breakage and forming C at the tail end + The reaction with water eventually degrades into oligosaccharides and monosaccharides, while protons are released, which continue to participate in new hydrolysis reactions. The common methods for pretreatment of dissolving pulp are: dilute acid pretreatment, saturated steam pretreatment, high-temperature hot water pretreatment and the like. The main components of the pre-hydrolysis liquid of the dissolving pulp comprise oligosaccharide, monosaccharide, lignin, a small amount of aldehyde substances and organic acid. Preferably, the polysaccharide content in the dissolving pulp prehydrolysis liquid is 10-25g/L, the monosaccharide content is 12-18g/L, and the lignin content is 8-12g/L.
Preferably, the dissolving pulp prehydrolysis liquid needs to be evaporated and concentrated, and the solid content after concentration is 10-20wt%.
Further, the starch is selected from one or more of cassava starch, corn starch, potato starch and wheat starch.
Further, the acid catalyst is selected from one or more of sulfuric acid, hydrochloric acid, acetic acid, citric acid and oxalic acid.
Further, the inorganic base is selected from one or more of sodium hydroxide, barium hydroxide and potassium hydroxide.
Further, the dialdehyde is selected from one or more of glyoxal, glutaraldehyde, succinaldehyde and o-phthalaldehyde.
Further, the initiator is selected from one or more of sodium persulfate, potassium persulfate, ammonium persulfate, hydrogen peroxide, tert-butyl hydroperoxide, cyclohexanone peroxide, benzoyl peroxide, azo initiators, cerium ammonium nitrate and percarbonate, preferably any one of potassium persulfate, ammonium persulfate and cerium ammonium nitrate.
Further, the stabilizer is selected from one or more of sodium thiosulfate, sodium bisulfite, sodium phosphite and sodium sulfite.
Further, the complexing agent is ethylenediamine tetraacetic acid salt, preferably disodium ethylenediamine tetraacetic acid and/or tetrasodium ethylenediamine tetraacetic acid.
The second aspect of the invention provides a preparation method of an interlayer reinforcing agent for papermaking, wherein the raw material of the interlayer reinforcing agent for papermaking adopts the raw material composition; the preparation method comprises the following steps:
s1, adding starch and a complexing agent into pre-hydrolyzed solution of dissolving pulp, heating to 50-60 ℃, adding an acid catalyst, dropwise adding a mixture of dialdehyde and water, and after dropwise adding, carrying out heat preservation reaction at the temperature for 60-120min to obtain a material A;
s2, adding inorganic base into the material A, dropwise adding an initiator and acrylamide at the temperature of 50-60 ℃, keeping the temperature for reaction for 60-90min after completing dropwise adding, adding a stabilizer, and cooling to room temperature to obtain the yellow liquid interlayer reinforcing agent for papermaking.
The third aspect of the present invention is to provide an interlaminar reinforcing agent for papermaking, which is prepared by the preparation method of the interlaminar reinforcing agent for papermaking.
The components of oligosaccharide, monosaccharide and the like in the pre-hydrolysis liquid of the dissolving pulp contain hydroxyl, the hydroxyl and aldehyde are subjected to polycondensation reaction under the action of an acid catalyst, and an initiator is used for initiating starch and graft copolymerization of oligosaccharide, monosaccharide, lignin and monomers in the dissolving pulp after alkali neutralization, so that macromolecules with a certain space network structure and multiple reaction groups are formed, and the function of a reinforcing agent is exerted. The complexing agent is added in the polycondensation reaction, so that metal ions in the reaction system can be complexed, and the stability of the whole reaction system is improved.
The interlayer reinforcing agent for papermaking, which is prepared by the invention, takes pulping waste liquid with wide renewable sources as a main raw material, can realize efficient utilization of resources, and changes waste into valuable; the pulping waste liquid is cheap and easy to obtain and is sufficiently supplied; the interlaminar reinforcing agent for papermaking prepared from the pulping waste liquid has the advantages of relatively simple raw material formula, simple preparation steps and easy operation, and the interlaminar reinforcing agent used for spraying paper can effectively improve the internal combination between fibers and the ring crush value of a paper sample.
Detailed Description
The following description is provided to disclose the invention so as to enable any person skilled in the art to practice the invention. The preferred embodiments described below are intended as examples only and are not intended to limit the scope of the invention, as other obvious modifications will occur to those skilled in the art. The basic principles of the invention, as defined in the following description, may be applied to other embodiments, variations, modifications, equivalents, and other technical solutions without departing from the spirit and scope of the invention.
The apparatus or raw materials in the present invention are not indicated by manufacturers, and are all conventional commercial apparatuses or raw materials. The main instruments and raw materials used in the following examples were as follows:
raw materials: the dissolving pulp prehydrolysis liquid is prepared by adopting a first-stage high-temperature water boiling pretreatment process of a dissolving pulp production line of a paper mill, wherein the content of oligosaccharide is 14.0-15.2 g/L, the content of monosaccharide is 12.3-13.2g/L, and the content of lignin is 8.4-9.0 g/L.
If the detection indexes related to the embodiment of the invention are not mentioned, the detection is carried out by adopting a conventional detection method or instrument in the field, and the specific index detection method is as follows:
the interlayer bonding strength adopts an IBT interlayer bonding strength tester;
the ring pressure index is measured by a DCP-KY3000 ring pressure index tester.
Example 1
(1) Taking 400g of dissolving pulp prehydrolysis liquid into a 1L glass reaction kettle, stirring and dispersing, adding 80g of corn starch and 0.8g of tetrasodium ethylene diamine tetraacetate into the reaction kettle, stirring and dispersing, simultaneously starting heating, raising the temperature to 50 ℃, adding 4g of 1mol/L sulfuric acid, dropwise adding a liquid mixed by 16g of glutaraldehyde and 20g of water, wherein the dropwise adding time is 40min, and after the dropwise adding is finished, keeping the temperature for 120min to prepare a material A;
(2) Adding 8g of potassium hydroxide into the material A prepared in the step (1), respectively dropwise adding 80g of 10% ammonium persulfate solution and 40g of acrylamide with 60g of water mixture, dropwise adding sodium persulfate for 80min, dropwise adding acrylamide mixed solution for 60min, reacting at 50 ℃, preserving heat for 90min after all dropwise adding, adding 4g of sodium thiosulfate after finishing preserving heat, and cooling to room temperature to obtain light yellow interlayer reinforcing agent liquid.
Example 2
(1) Taking 400g of dissolving pulp prehydrolysis liquid into a 1L glass reaction kettle, stirring and dispersing, adding 40g of cassava starch and 0.4g of disodium ethylene diamine tetraacetate into the reaction kettle, stirring and dispersing, simultaneously starting to heat up, raising the temperature to 60 ℃, adding 2g of 1mol/L hydrochloric acid, dropwise adding a liquid mixed by 10g of glyoxal and 10g of water, wherein the dropwise adding time is 20min, and keeping the temperature for 90min after dropwise adding is completed to prepare a material A;
(2) Adding 4g of sodium hydroxide into the material A prepared in the step (1), respectively dropwise adding 32g of 10% sodium persulfate solution and 20g of acrylamide and 20g of water mixture, dropwise adding sodium persulfate for 60min, dropwise adding acrylamide mixed solution for 40min, reacting at 55 ℃, preserving heat for 60min after all dropwise adding, adding 3g of sodium thiosulfate after finishing preserving heat, and cooling to room temperature to obtain faint yellow interlayer reinforcing agent liquid.
Example 3
(1) Taking 400g of dissolving pulp prehydrolysis liquid into a 1L glass reaction kettle, stirring and dispersing, adding 20g of corn starch, 20g of potato starch and 0.7g of disodium ethylene diamine tetraacetate into the reaction kettle, stirring and dispersing, simultaneously starting heating, raising the temperature to 55 ℃, adding 4g of 2mol/L acetic acid, dropwise adding a liquid mixed by 12g of glutaraldehyde and 12g of water, wherein the dropwise adding time is 30min, and preserving heat for 90min after dropwise adding is completed to prepare a material A;
(2) And (2) adding 5g of sodium hydroxide into the material A prepared in the step (1), respectively dropwise adding 60g of 10% benzoyl peroxide and 30g of acrylamide into 30g of a water mixture, dropwise adding sodium persulfate for 60min, dropwise adding an acrylamide mixed solution for 50min, keeping the reaction temperature at 60 ℃, keeping the temperature for 90min after all dropwise adding, adding 2g of sodium bisulfite after the temperature is kept, and cooling to room temperature to obtain a light yellow interlayer reinforcing agent liquid.
Example 4
(1) Taking 400g of dissolving pulp prehydrolysis liquid into a 1L glass reaction kettle, stirring and dispersing, adding 60g of corn starch and 0.4g of tetrasodium ethylene diamine tetraacetate into the reaction kettle, stirring and dispersing, simultaneously starting heating, raising the temperature to 60 ℃, adding 4g of 2mol/L citric acid, dropwise adding a liquid mixed by 10g of o-phthalaldehyde and 20g of water, wherein the dropwise adding time is 30min, and preserving heat for 60min after dropwise adding is finished to prepare a material A;
(2) And (2) adding 4g of barium hydroxide into the material A prepared in the step (1), respectively dropwise adding 80g of 10% ammonium persulfate solution and 30g of acrylamide and 20g of water mixture, dropwise adding sodium persulfate for 60min, dropwise adding acrylamide mixed solution for 50min, reacting at the temperature of 60 ℃, preserving heat for 90min after all dropwise adding is finished, adding 4g of sodium sulfite after the heat preservation is finished, and cooling to room temperature to obtain light yellow interlayer reinforcing agent liquid.
Comparative example 1
The difference from example 1 is that the hydrolysis solution of the dissolved pulp is replaced with pure water in step (1), and the other condition parameters are the same as those in example 1.
Comparative example 2
Compared with the example 1, the difference is that in the step (1), sulfuric acid is not added, and other condition parameters are the same as the example 1.
Comparative example 3
Compared with the example 1, the difference is that no glutaraldehyde is added in the step (1), and other condition parameters are the same as the example 1.
Comparative example 4
Compared with the example 1, the difference is that no acrylamide is added in the step (2), and other condition parameters are the same as the example 1.
Application examples
Weighing quantitative flour paste, making into sheet, and transferring with absorbent paper; adding 10ppm of purple dye into the bottom slurry, dyeing, and forming into sheets; transferring the bottom pulp pattern from the surface pulp pattern, squeezing, drying, balancing water content, and testing interlayer bonding strength and ring crush.
Drying and balancing each sample paper sample by a glazing machine (setting 150 ℃, actually measuring temperature is about 110 ℃), weighing and quantifying, and detecting internal bonding strength and ring crush.
The control was a commercially available spray starch.
The specific measurement results are shown in table 1:
TABLE 1 paper pattern test index
It can be seen from the data in table 1 that the interlayer reinforcing agents prepared in examples 1 to 4 are effective in improving the ring crush index and the internal bond strength, as compared to the reinforcing agents prepared in comparative examples 1 to 4.
It will be appreciated by persons skilled in the art that the above examples are given by way of illustration only and are not limiting of the invention. The objects of the present invention have been fully and effectively accomplished. The functional and structural principles of the present invention have been shown and described in the examples, and any variations or modifications of the embodiments of the present invention may be made without departing from the principles.
Claims (8)
1. The raw material composition of the interlayer reinforcing agent for papermaking is characterized by comprising the following components in parts by weight: 100 parts of dissolving pulp prehydrolysis liquid, 10-20 parts of starch, 5-10 parts of acrylamide, 0.5-1 part of acid catalyst, 1-2 parts of inorganic base, 2-4 parts of dialdehyde, 0.5-2 parts of initiator, 1-2 parts of stabilizer and 0.1-0.2 part of complexing agent; the dissolving pulp prehydrolysis liquid contains oligosaccharide in 10-25g/L, monosaccharide in 12-18g/L and lignin in 8-12g/L.
2. The raw material composition of the interlayer reinforcing agent for papermaking according to claim 1, wherein the starch is one or more selected from the group consisting of tapioca native starch, corn starch, potato starch, wheat starch; the acid catalyst is selected from one or more of sulfuric acid, hydrochloric acid, acetic acid, citric acid and oxalic acid; the inorganic base is selected from one or more of sodium hydroxide, barium hydroxide and potassium hydroxide; the dialdehyde is one or more selected from glyoxal, glutaraldehyde, succinaldehyde and o-phthalaldehyde.
3. The stock composition of an interlayer reinforcing agent for papermaking according to claim 1, wherein the initiator is one or more selected from the group consisting of sodium persulfate, potassium persulfate, ammonium persulfate, hydrogen peroxide, t-butyl hydroperoxide, cyclohexanone peroxide, benzoyl peroxide, azo-type initiator, ammonium cerium nitrate and percarbonate; the stabilizer is selected from one or more of sodium thiosulfate, sodium bisulfite, sodium phosphite and sodium sulfite.
4. The raw material composition of an interlaminar reinforcing agent for papermaking according to claim 1, characterized in that the complexing agent is ethylenediamine tetraacetate.
5. The preparation method of the interlayer reinforcing agent for papermaking is characterized by comprising the following steps:
s1, adding starch and a complexing agent into pre-hydrolysis liquid of dissolving pulp, heating to 50-60 ℃, adding an acid catalyst, dropwise adding a mixture of dialdehyde and water, and after dropwise adding is finished, keeping the temperature at the temperature for reaction for 60-120min to obtain a material A;
s2, adding inorganic base into the material A, dropwise adding an initiator and acrylamide at the temperature of 50-60 ℃, keeping the temperature for reaction for 60-90min after completing dropwise adding, adding a stabilizer, and cooling to room temperature to obtain a yellow liquid interlayer reinforcing agent for papermaking;
the dissolving pulp prehydrolysis liquid contains oligosaccharide in 10-25g/L, monosaccharide in 12-18g/L and lignin in 8-12g/L.
6. The method of claim 5, wherein the starch is selected from one or more of raw tapioca starch, corn starch, potato starch, wheat starch; the acid catalyst is selected from one or more of sulfuric acid, hydrochloric acid, acetic acid, citric acid and oxalic acid; the inorganic base is selected from one or more of sodium hydroxide, barium hydroxide and potassium hydroxide; the dialdehyde is one or more selected from glyoxal, glutaraldehyde, succinaldehyde and o-phthalaldehyde; the initiator is selected from one or more of sodium persulfate, potassium persulfate, ammonium persulfate, hydrogen peroxide, tert-butyl hydroperoxide, cyclohexanone peroxide, benzoyl peroxide, azo initiators, ammonium ceric nitrate and percarbonate; the stabilizer is selected from one or more of sodium thiosulfate, sodium bisulfite, sodium phosphite and sodium sulfite.
7. The method of claim 5, wherein the complexing agent is ethylenediaminetetraacetate.
8. An interlaminar reinforcing agent for papermaking prepared by the method of any one of claims 5 to 7.
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Citations (4)
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|---|---|---|---|---|
| CN103726379A (en) * | 2014-01-09 | 2014-04-16 | 齐鲁工业大学 | Application of modified nano-microcrystalline cellulose serving as papermaking strengthening agent |
| CN109535319A (en) * | 2018-11-07 | 2019-03-29 | 济宁明升新材料有限公司 | A kind of environmentally friendly drying strengthening agent and preparation method thereof |
| CN111172808A (en) * | 2020-02-11 | 2020-05-19 | 九洲生物技术（苏州）有限公司 | Reinforcing agent for spraying between paper layers and preparation method thereof |
| CN113089368A (en) * | 2021-03-29 | 2021-07-09 | 上海昶法新材料有限公司 | Reinforcing agent for natural polymer modified paper interlayer spraying and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3512995A2 (en) * | 2016-09-16 | 2019-07-24 | Basf Se | Methods of modifying pulp comprising cellulase enzymes and products thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103726379A (en) * | 2014-01-09 | 2014-04-16 | 齐鲁工业大学 | Application of modified nano-microcrystalline cellulose serving as papermaking strengthening agent |
| CN109535319A (en) * | 2018-11-07 | 2019-03-29 | 济宁明升新材料有限公司 | A kind of environmentally friendly drying strengthening agent and preparation method thereof |
| CN111172808A (en) * | 2020-02-11 | 2020-05-19 | 九洲生物技术（苏州）有限公司 | Reinforcing agent for spraying between paper layers and preparation method thereof |
| CN113089368A (en) * | 2021-03-29 | 2021-07-09 | 上海昶法新材料有限公司 | Reinforcing agent for natural polymer modified paper interlayer spraying and preparation method thereof |
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