CN115467182A - Pretreatment process for paper pulp production raw materials - Google Patents
Pretreatment process for paper pulp production raw materials Download PDFInfo
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- CN115467182A CN115467182A CN202211011121.7A CN202211011121A CN115467182A CN 115467182 A CN115467182 A CN 115467182A CN 202211011121 A CN202211011121 A CN 202211011121A CN 115467182 A CN115467182 A CN 115467182A
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- impregnation
- pulp production
- waste liquid
- pretreatment
- liquid
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- 238000000034 method Methods 0.000 title claims abstract description 61
- 230000008569 process Effects 0.000 title claims abstract description 52
- 239000002994 raw material Substances 0.000 title claims abstract description 35
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 31
- 229920001131 Pulp (paper) Polymers 0.000 title claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 114
- 239000002699 waste material Substances 0.000 claims abstract description 67
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 66
- 238000005470 impregnation Methods 0.000 claims abstract description 65
- 239000003513 alkali Substances 0.000 claims abstract description 44
- 238000011084 recovery Methods 0.000 claims abstract description 31
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 239000007787 solid Substances 0.000 claims abstract description 28
- 238000007598 dipping method Methods 0.000 claims abstract description 26
- 239000000203 mixture Substances 0.000 claims abstract description 25
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims abstract description 24
- 235000011121 sodium hydroxide Nutrition 0.000 claims abstract description 22
- 238000001556 precipitation Methods 0.000 claims abstract description 19
- 238000000926 separation method Methods 0.000 claims abstract description 15
- 239000002023 wood Substances 0.000 claims abstract description 14
- 239000013049 sediment Substances 0.000 claims abstract description 12
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 7
- 239000008394 flocculating agent Substances 0.000 claims abstract description 7
- 230000002209 hydrophobic effect Effects 0.000 claims description 15
- 239000003795 chemical substances by application Substances 0.000 claims description 13
- 238000005185 salting out Methods 0.000 claims description 13
- 239000003999 initiator Substances 0.000 claims description 12
- 229910021645 metal ion Inorganic materials 0.000 claims description 12
- 239000003607 modifier Substances 0.000 claims description 12
- 238000007348 radical reaction Methods 0.000 claims description 12
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 11
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 11
- 239000001632 sodium acetate Substances 0.000 claims description 11
- 235000017281 sodium acetate Nutrition 0.000 claims description 11
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 10
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 10
- 150000003254 radicals Chemical class 0.000 claims description 8
- 238000004064 recycling Methods 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 6
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 6
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 6
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 claims description 6
- 239000011780 sodium chloride Substances 0.000 claims description 5
- KSCAZPYHLGGNPZ-UHFFFAOYSA-N 3-chloropropyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)CCCCl KSCAZPYHLGGNPZ-UHFFFAOYSA-N 0.000 claims description 4
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 4
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 3
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 3
- OXYZDRAJMHGSMW-UHFFFAOYSA-N 3-chloropropyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)CCCCl OXYZDRAJMHGSMW-UHFFFAOYSA-N 0.000 claims description 3
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 3
- -1 alkenyl succinic anhydride Chemical compound 0.000 claims description 3
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 3
- 125000000751 azo group Chemical group [*]N=N[*] 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- 229920002401 polyacrylamide Polymers 0.000 claims description 3
- 235000011056 potassium acetate Nutrition 0.000 claims description 3
- 239000001103 potassium chloride Substances 0.000 claims description 3
- 235000011164 potassium chloride Nutrition 0.000 claims description 3
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 3
- 229940014800 succinic anhydride Drugs 0.000 claims description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 2
- 125000002091 cationic group Chemical group 0.000 claims description 2
- 159000000021 acetate salts Chemical class 0.000 claims 1
- 229920002488 Hemicellulose Polymers 0.000 abstract description 46
- 239000000243 solution Substances 0.000 abstract description 15
- 239000007853 buffer solution Substances 0.000 abstract description 7
- 238000003381 deacetylation reaction Methods 0.000 abstract description 5
- DGPIGKCOQYBCJH-UHFFFAOYSA-M sodium;acetic acid;hydroxide Chemical compound O.[Na+].CC([O-])=O DGPIGKCOQYBCJH-UHFFFAOYSA-M 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 3
- 239000012527 feed solution Substances 0.000 abstract description 2
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 abstract 2
- 125000002777 acetyl group Chemical group [H]C([H])([H])C(*)=O 0.000 description 21
- 238000004537 pulping Methods 0.000 description 14
- 239000000126 substance Substances 0.000 description 14
- 239000005416 organic matter Substances 0.000 description 12
- 238000003756 stirring Methods 0.000 description 12
- 239000002244 precipitate Substances 0.000 description 11
- 238000005259 measurement Methods 0.000 description 10
- 241000219000 Populus Species 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 238000001914 filtration Methods 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- 239000000835 fiber Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000005189 flocculation Methods 0.000 description 3
- 230000016615 flocculation Effects 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000000967 suction filtration Methods 0.000 description 3
- 230000001502 supplementing effect Effects 0.000 description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000001110 calcium chloride Substances 0.000 description 2
- 229910001628 calcium chloride Inorganic materials 0.000 description 2
- 210000002421 cell wall Anatomy 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000007822 coupling agent Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000004811 liquid chromatography Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000007127 saponification reaction Methods 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 229910020175 SiOH Inorganic materials 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 230000003311 flocculating effect Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 239000011121 hardwood Substances 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 150000002432 hydroperoxides Chemical class 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 238000006011 modification reaction Methods 0.000 description 1
- 229920001542 oligosaccharide Polymers 0.000 description 1
- 150000002482 oligosaccharides Chemical class 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C1/00—Pretreatment of the finely-divided materials before digesting
- D21C1/06—Pretreatment of the finely-divided materials before digesting with alkaline reacting compounds
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C1/00—Pretreatment of the finely-divided materials before digesting
Abstract
The application discloses paper pulp raw materials for production preliminary treatment technology includes the following steps: adding caustic soda into the wood chip raw material to carry out impregnation treatment to obtain cold alkali impregnation waste liquid; soluble acetate is also added in the process of dipping treatment; adding a pretreatment reagent into the cold alkali dipping waste liquid for pretreatment reaction, and obtaining a first mixture system after the pretreatment reaction is finished; adding a flocculating agent into the first mixture system for precipitation reaction to obtain a second mixture system after the precipitation reaction is finished; carrying out solid-liquid separation on the second mixture system to obtain solid organic sediment and alkaline recovery liquid; the alkaline recovery solution is recycled as the impregnation feed solution for the impregnation treatment. The pretreatment process can form an acetate-sodium hydroxide buffer system, can inhibit deacetylation reaction of hemicellulose in the dipping process, improves the content of acetyl hemicellulose in waste liquid, and can obtain acetyl hemicellulose with high application value in high yield after solid-liquid separation.
Description
Technical Field
The application belongs to the technical field of paper pulp production, and particularly relates to a paper pulp production raw material pretreatment process.
Background
Cold soda pulping is a high-yield pulping technology for impregnating plant fiber raw materials with alkaline solution. Caustic soda is used for removing part of hemicellulose and a small amount of lignin in the wood chips, softening intercellular layers, reducing the energy consumption of subsequent mechanical treatment for separating fibers, and obtaining a paper pulp product meeting the paper making requirement. The traditional cold alkali pulping adopts a caustic soda solution with higher concentration to carry out dipping treatment on raw materials, and the caustic soda is utilized to break the hydrogen bond connection between the hemicellulose and the cellulose, so as to promote the alkali-soluble hemicellulose to be dissolved out. Meanwhile, hemicellulose acetyl in the wood raw material falls off through saponification reaction, so that the waste liquid contains a large amount of acetic acid and the acetyl-removed hemicellulose obtained after saponification reaction. The production process causes the difference between the hemicellulose structure contained in the waste liquid of the traditional cold-alkali pulping process and the in-situ hemicellulose in the wood raw material, and acetyl groups with different contents have different influences on the modification reaction and the application field of the hemicellulose from the comprehensive utilization value of the hemicellulose, thereby providing richer selectivity for the industrial application of the hemicellulose. Therefore, the pretreatment process of the paper pulp production raw material is developed, on the basis of meeting the quality requirement of conventional pulping production, the controllable structure of the acetyl functional group of the hemicellulose byproduct in the pulping waste liquid is realized by changing the process elements, the development of the biomass refining technology based on the traditional pulping and papermaking platform is further promoted, the comprehensive utilization level of plant fiber resources is improved, and the pollution control and low-carbon development of the pulping and papermaking industry are promoted.
Disclosure of Invention
The application aims to overcome the defects of at least one aspect of the prior art, and provides a paper pulp production raw material pretreatment process to solve the technical problems that acetyl hemicellulose with high application value cannot be obtained in high yield in the existing paper pulp production process, and pulping waste liquid cannot be reasonably utilized.
In order to achieve the above object, the present application provides a pulp production raw material pretreatment process, comprising the steps of:
adding caustic soda into the wood chip raw material for impregnation treatment to obtain cold alkali impregnation waste liquid; soluble acetate is also added in the dipping treatment process;
adding a pretreatment reagent into the cold alkali dipping waste liquid for pretreatment reaction, and obtaining a first mixture system after the pretreatment reaction is finished;
adding a flocculating agent into the first mixture system for precipitation reaction, and obtaining a second mixture system after the precipitation reaction is finished;
carrying out solid-liquid separation on the second mixture system to obtain a solid organic sediment and an alkaline recovery solution;
and recycling the alkaline recovery liquid to be used as the impregnation liquid of the impregnation treatment.
Further, the soluble acetate is at least one of sodium acetate and potassium acetate.
Further, in the impregnation treatment process, the mass ratio of the wood chip raw material to the caustic soda is 1:2 to 1:10; the addition amount of the acetate is 0.01 g/L-10 g/L.
Further, the pretreatment reagent is at least one of a hydrophobic modifier, a radical reaction initiator and a metal ion salting-out agent.
Further, the hydrophobic modifier is at least one of silane coupling agent, 1, 2-alkylene oxide and alkenyl succinic anhydride; and/or
The free radical reaction initiator is at least one of persulfate, azo compounds and hydroperoxide; and/or
The metal ion salting-out agent is at least one of sodium chloride, potassium chloride and lithium chloride.
Further, the silane coupling agent is at least one of gamma-chloropropyl triethoxysilane, gamma-chloropropyl methyl dichlorosilane, gamma-chloropropyl trimethoxysilane, gamma-aminopropyl triethoxysilane and gamma-aminopropyl trimethoxysilane; and/or
The persulfate is at least one of potassium persulfate, sodium persulfate and ammonium persulfate.
Further, the flocculating agent is at least one of polyaluminium chloride, cationic polyacrylamide and ferric trichloride.
Further, the dosage of the hydrophobic modifier is 10-20 g/L; and/or
The adding amount of the free radical reaction initiator is 5-15 g/L; and/or
The dosage of the metal ion salting-out agent is 5 to 15g/L.
Furthermore, the adding amount of the flocculant is 0.1-0.4 g/L.
Furthermore, the temperature of the dipping treatment is 20-90 ℃, and the dipping time is 2-6 h.
Compared with the prior art, the method has the following technical effects:
according to the paper pulp production raw material pretreatment process, soluble acetate is added in the dipping treatment process, the soluble acetate can form an acetate-sodium hydroxide buffer system with caustic soda in the dipping treatment system, the existence of the buffer system can inhibit the deacetylation reaction of hemicellulose in the dipping process, so that the hemicellulose in the dipped waste liquid can exist in the form of acetyl hemicellulose in a large amount, the content of acetyl hemicellulose in the waste liquid is improved, and the acetyl hemicellulose with high application value can be obtained in a high yield after solid-liquid separation.
On the other hand, the pretreatment process of the paper pulp production raw material recycles the alkaline recovery liquid as the impregnation liquid for impregnation treatment, on one hand, acetate components in the alkaline recovery liquid are continuously accumulated in the system in the recycling process, and the accumulated acetate can further inhibit the deacetylation reaction of hemicellulose in the impregnation process, so that the high-content acetyl hemicellulose can be obtained; on the other hand, the recycling of the alkaline recovery solution can reduce the consumption of new alkali, fully utilize chemical resources in the waste liquid and reduce the influence of the pulping waste liquid on the environment.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present application more clearly apparent, the present application is further described in detail below with reference to the embodiments. It should be understood that the specific embodiments described herein are merely illustrative of and not restrictive on the broad application.
In this application, the term "and/or" describes an association relationship of associated objects, meaning that there may be three relationships, e.g., a and/or B, which may mean: a is present alone, A and B are present simultaneously, and B is present alone. Wherein A and B can be singular or plural. The character "/" generally indicates that the former and latter associated objects are in an "or" relationship.
In the present application, "at least one" means one or more, "a plurality" means two or more. "at least one of the following" or similar expressions refer to any combination of these items, including any combination of the singular or plural items. For example, "at least one (a), b, or c", or "at least one (a), b, and c", may each represent: a, b, c, a-b (i.e., a and b), a-c, b-c, or a-b-c, wherein a, b, and c may be single or plural, respectively.
It should be understood that, in various embodiments of the present application, the sequence numbers of the foregoing processes do not imply an execution sequence, some or all of the steps may be executed in parallel or executed sequentially, and the execution sequence of each process should be determined by its function and inherent logic, and should not limit the implementation process of the embodiments of the present application.
The terminology used in the embodiments of the present application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used in the examples of this application and the appended claims, the singular forms "a", "an", and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
The weight of the related components mentioned in the description of the embodiments of the present application may not only refer to the specific content of each component, but also represent the proportional relationship of the weight among the components, and therefore, the content of the related components is scaled up or down within the scope disclosed in the description of the embodiments of the present application as long as it is scaled up or down according to the description of the embodiments of the present application. Specifically, the mass described in the specification of the examples of the present application may be a mass unit known in the chemical field such as μ g, mg, g, kg, etc.
The terms "first" and "second" are used for descriptive purposes only and are used for distinguishing purposes such as substances from one another and are not to be construed as indicating or implying relative importance or to implicitly indicate the number of technical features indicated. For example, a first XX may also be referred to as a second XX, and similarly, a second XX may also be referred to as a first XX, without departing from the scope of embodiments of the present application. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature.
The embodiment of the application provides a paper pulp production raw material pretreatment process, which comprises the following steps:
(1) Adding caustic soda into the wood chip raw material for impregnation treatment to obtain cold alkali impregnation waste liquid; soluble acetate is also added in the process of dipping treatment;
(2) Adding a pretreatment reagent into the cold alkali dipping waste liquid for pretreatment reaction to obtain a first mixture system after the pretreatment reaction is finished;
(3) Adding a flocculating agent into the first mixture system for precipitation reaction to obtain a second mixture system after the precipitation reaction is finished;
(4) Carrying out solid-liquid separation on the second mixture system to obtain a solid organic sediment and an alkaline recovery solution;
(5) The alkaline recycle solution is recycled as the impregnation feed solution for the impregnation treatment.
According to the paper pulp production raw material pretreatment process, soluble acetate is added in the dipping treatment process, the soluble acetate can form an acetate-sodium hydroxide buffer system with caustic soda in the dipping treatment system, the existence of the buffer system can inhibit the deacetylation reaction of hemicellulose in the dipping process, the hemicellulose in the dipped waste liquid can exist in the form of acetyl hemicellulose, the acetyl hemicellulose content in the waste liquid is improved, and the acetyl hemicellulose with high application value can be obtained in a high yield after solid-liquid separation.
On the other hand, in the paper pulp production raw material pretreatment process, the alkaline recovery liquid is recycled as the impregnation liquid for impregnation treatment, on one hand, acetate components in the alkaline recovery liquid are continuously accumulated in a system in the recycling process, and the accumulated acetate can further inhibit the deacetylation reaction of hemicellulose in the impregnation process, so that high-content acetyl hemicellulose can be obtained; on the other hand, the recycling of the alkaline recovery solution can reduce the consumption of new alkali, fully utilize chemical resources in the waste liquid and reduce the influence of the pulping waste liquid on the environment.
In the present embodiment, the soluble acetate in the step (1) may be at least one of sodium acetate and potassium acetate. The soluble acetate to be added in the step (1) may be an aqueous solution of pure acetate or a mixture system containing acetate.
In the embodiment of the present application, in the impregnation treatment process in the step (1), the mass ratio of the wood chip raw material to the caustic soda is 1:2 to 1:10, namely adding 2-10L of liquid caustic soda into each kilogram of wood chip raw materials, wherein the concentration of the liquid caustic soda is 20-60 g/L; the addition amount of the acetate is 0.01g/L to 10g/L, namely 0.01g to 10g of acetate is added into each liter of impregnation liquid. The wood chip raw material of the present embodiment refers to hardwood, and specifically, may be poplar wood chips. The temperature of the dipping treatment can be controlled to be 20-90 ℃, and the dipping time is 2-6 h.
The pretreatment reagent in the step (2) is at least one of a hydrophobic modifier, a free radical reaction initiator and a metal ion salting-out agent. The hydrophobic modifier can perform hydrophobic modification on organic matters in the waste liquid, and weaken the compatibility and the dispersibility of the modified organic matters in the waste liquid, so that the organic matters after the hydrophobic modification are more easily precipitated from a waste liquid system.
In the embodiment of the present application, the hydrophobic modifier may be selected from at least one of a silane coupling agent, a 1, 2-alkylene oxide, and alkenyl succinic anhydride. Specifically, the silane coupling agent can be at least one of gamma-chloropropyl triethoxysilane, gamma-chloropropyl methyl dichlorosilane, gamma-chloropropyl trimethoxysilane, gamma-aminopropyl triethoxysilane and gamma-aminopropyl trimethoxysilane. In the specific embodiment of the application, a silane coupling agent is used as a hydrophobic modifier of the organic matter. The dosage of the hydrophobic modifier is 10-20 g/L, namely 10-20 g of hydrophobic modifier is added into each liter of waste liquid, and the preferred dosage is 15g/L. After adding the silane coupling agent, in the pretreatment reaction process,alkoxy- (OR) in silane coupling agent 3 Firstly, the organic matter in the waste liquid reacts with water in the waste liquid or water on the surface of an organic matter containing hydroxyl to generate silicon hydroxyl (SiOH-), then the molecules of the coupling agent generate a siloxane Si-O-Si with lower polymerization degree through dehydration condensation reaction among partial silicon hydroxyl, meanwhile, the silicon hydroxyl still contains abundant silicon hydroxyl SiOH < - > on the structure, and the silicon hydroxyl and the hydroxyl on the surface of the organic matter form hydrogen bond action, and then the hydroxyl is further dehydrated to enable the molecules of the coupling agent and the surface of the organic matter to form stable covalent bond, so that the organic matter in the waste liquid is divided by the silane coupling agent, one end with the hydroxyl is tightly combined with the silane coupling agent, and the other end is keyed in a hydrophobic organic group to enable the surface property of organic matter particles to change, the surface energy is reduced, the compatibility and the dispersibility of the organic matter in a water phase system are weakened, and the subsequent flocculation precipitation treatment of the organic matter is facilitated.
In this embodiment, a radical reaction initiator may also be added to the cold alkali impregnation effluent to precipitate the organics in the effluent. The free radical reaction initiator can make organic matter molecules in the waste liquid cross-linked with each other and converted into macromolecular organic matter with lower water solubility, thereby being beneficial to the subsequent flocculation and precipitation treatment. In the embodiment of the present application, the radical reaction initiator may be at least one selected from persulfates, azo compounds, and hydroperoxides. Specifically, in the embodiment of the application, a persulfate is used as an initiator of the radical reaction, and the persulfate can be selected from at least one of potassium persulfate, sodium persulfate and ammonium persulfate. The amount of the radical reaction initiator added is 5 to 15g/L, preferably 8g/L. After persulfate is added into the cold alkali impregnation waste liquid, the persulfate and organic substances with hydroxyl in the waste liquid are subjected to a crosslinking reaction, and free radicals generated by the persulfate can crosslink the organic substances into macromolecular organic substances with lower water solubility.
In the embodiment of the application, a metal ion salting-out agent can be added into the cold alkali impregnation waste liquid to promote the settling separation of organic matters in the waste liquid. After the metal ion salting-out agent is added, in the salting-out process of cations, due to the strong hydration action of the metal ion salting-out agent in an aqueous solution, a large amount of free water molecules can be attracted, and the concentration of the free water molecules in the organic aqueous solution is reduced, so that the organic molecules in the waste liquid are promoted to flocculate, and the subsequent flocculation precipitation treatment is facilitated. In the embodiment of the present application, the metal ion salting-out agent may be at least one of sodium chloride, potassium chloride and lithium chloride. The addition amount of the metal ion salting-out agent is 5 to 15g/L, preferably 8g/L.
In the embodiment of the application, the temperature of the pretreatment reaction can be controlled to be 20-90 ℃ and the time is 30-90 min. Under the pretreatment reaction condition, organic matter components in the waste liquid can be quickly and efficiently settled out.
In the step (3), the flocculant in the embodiment of the present application may be at least one selected from polyaluminium chloride, anionic polyacrylamide, and ferric chloride. And (3) flocculating suspended particles in the waste liquid by adding a flocculating agent into the first mixture system pretreated by the step (2) to promote the suspended particles to be rapidly settled from the waste liquid. The addition amount of the flocculating agent can be selected from 0.1-0.4 g/L, and is preferably 0.25g/L. The precipitation reaction can be carried out at room temperature, and the time of the precipitation reaction can be regulated and controlled according to the content of organic matters in the waste liquid.
In the step (4), after solid-liquid separation, the solid organic sediments can be directly recycled as high value-added products, such as packaging materials, papermaking additives, decorative coatings, and foods or biological medicines; and the pH value of the alkaline recovery liquid is 11.8-13, namely the concentration of the alkali in the alkaline recovery liquid is still kept at a higher pH value level, so that the alkaline recovery liquid can be directly recovered and recycled as the impregnation liquid for impregnation treatment, and the consumption of new alkali is reduced.
The embodiment of the application firstly provides that the acetate-sodium hydroxide buffer system is utilized to pretreat the paper pulp production raw material, hemicellulose rich in acetyl is obtained in the cold alkali extraction process, and the complete extraction of the hemicellulose is realized.
The method for treating the waste liquid by using the pretreatment reagent composite flocculant in the embodiment of the application is simple and convenient in treatment method and simple in process conditions, greatly reduces the utilization rate of caustic soda, realizes the cyclic utilization of the caustic soda, and obtains organic matters with great application values.
In the primary alkaline recovery solution obtained by treatment in the embodiment of the application, the acetate ion content in the waste solution is saturated due to acetate pretreatment, ether bonds on fiber cell walls can be continuously destroyed, and the formation and dissolution of oligosaccharides in wood chip cell walls can be promoted.
A pulp production raw material pretreatment process of the embodiments of the present application is illustrated below by way of specific examples.
Example 1
The application embodiment 1 provides a paper pulp production raw material pretreatment process, which comprises the following steps:
(1) Adding 1kg of poplar chips into 5L of caustic soda solution with the concentration of 40g/L, adding a proper amount of sodium acetate to ensure that the addition amount of the sodium acetate in the impregnation liquid is 0.01g/L, and then carrying out primary impregnation treatment at the temperature of 30 ℃ for 6 hours; after the primary dipping treatment is finished, filtering out solid substances to obtain primary cold alkali dipping waste liquid;
(2) Adding 10g of gamma-chloropropyltriethoxysilane into the primary cold alkali impregnation waste liquid obtained in the step (1) to obtain a mixed solution A;
(3) Stirring the mixed solution A obtained in the step (1) at 35 ℃ to react for 60min to obtain a mixture system;
(4) And (4) dropwise adding 100mL of 0.1 g/mL polyaluminum chloride into the mixed system obtained in the step (3) under the stirring condition, wherein the stirring speed is 2000-4000 rpm, the stirring speed is 200-500 rpm after the addition is finished, and carrying out precipitation reaction for 10min.
(5) Performing suction filtration on the mixture system subjected to the precipitation reaction in the step (4), and separating solid from liquid to obtain a primary solid organic sediment and a primary alkaline recovery liquid;
(6) Adding 0.7kg of poplar chips into the primary alkaline recycling liquid obtained in the step (5), and supplementing a proper amount of caustic soda to ensure that the alkaline concentration in the impregnation liquid is 40g/L, and performing secondary impregnation treatment at the temperature of 30 ℃ for 6 hours; after the secondary impregnation treatment is finished, filtering solid substances to obtain secondary cold alkali impregnation waste liquid; and (3) repeating the operation steps (2) to (5) to obtain a secondary solid organic sediment and a secondary alkaline recovery solution.
The total hemicellulose and acetyl hemicellulose content in the primary solid organic precipitate of the examples of the present application was determined (by liquid chromatography) and the results are shown in the following table 1-1:
TABLE 1-1
The contents of the main components (the contents of the main components are measured by liquid chromatography) and the pH of the primary cold alkali impregnation waste liquid (before treatment) and the primary alkali recovery liquid (after treatment) in the examples of the present application were measured, and the measurement results are shown in the following tables 1 to 2:
tables 1 to 2
The "-" in table 1-2 represents that no corresponding component is detected, and it is seen from table 1-2 that the treatment method of the embodiment of the present application can precipitate more than 70% of the organic matters in the primary cold alkali impregnation waste liquid, i.e. can efficiently separate the organic matters from the waste liquid, and the pH of the waste liquid can still maintain a high alkaline level before and after separation.
Example 2
The embodiment 2 of the application provides a paper pulp production raw material pretreatment process, which comprises the following steps:
(1) Adding 1kg of poplar chips into 5L of caustic soda solution with the concentration of 40g/L, adding a proper amount of sodium acetate to ensure that the addition amount of the sodium acetate in the impregnation liquid is 0.1g/L, and then carrying out primary impregnation treatment at the temperature of 60 ℃ for 4 hours; after the primary dipping treatment is finished, filtering out solid substances to obtain primary cold alkali dipping waste liquid;
(2) Adding 10g of potassium persulfate into the primary cold alkali impregnation waste liquid obtained in the step (1) to obtain a mixed solution A;
(3) Stirring the mixed solution A obtained in the step (1) at 60 ℃ to react for 60min to obtain a mixture system;
(4) And (4) dropwise adding 100mL of 0.1 g/mL polyaluminum chloride into the mixed system obtained in the step (3) under the stirring condition, wherein the stirring speed is 2000-4000 rpm, the stirring speed is 200-500 rpm after the addition is finished, and carrying out precipitation reaction for 10min.
(5) Performing suction filtration on the mixture system subjected to the precipitation reaction in the step (4), and separating solid from liquid to obtain a primary solid organic sediment and a primary alkaline recovery liquid;
(6) Adding 0.7kg of poplar chips into the alkaline recovery liquid obtained in the step (5), supplementing a proper amount of caustic soda to ensure that the concentration of the alkali in the impregnation liquid is 40g/L, and carrying out secondary impregnation treatment at the temperature of 60 ℃ for 4 hours; after the secondary impregnation treatment is finished, filtering solid substances to obtain secondary cold alkali impregnation waste liquid; and (3) repeating the operation steps (2) to (5) to obtain a secondary solid organic sediment and a secondary alkaline recovery solution.
The total hemicellulose and acetyl hemicellulose contents in the primary solid organic precipitate of the examples of the present application were measured, and the measurement results are shown in the following table 2-1:
TABLE 2-1
The contents of main components and pH of the primary cold alkali impregnation waste liquid and the primary alkali recovery liquid in the examples of the present application were measured, and the measurement results are shown in the following tables 2 to 2:
tables 2 to 2
The "-" in table 2-2 represents that no corresponding component is detected, and it can be seen from table 2-2 that the treatment method in the embodiment of the present application can precipitate more than 70% of the organic matters in the primary cold alkali impregnation waste liquid, i.e. can efficiently separate the organic matters from the waste liquid, and the pH of the waste liquid can still maintain a high alkalinity level before and after separation.
Example 3
The application embodiment 3 provides a paper pulp production raw material pretreatment process, which comprises the following steps:
(1) Adding 1kg of poplar chips into 5L of caustic soda solution with the concentration of 40g/L, adding a proper amount of sodium acetate to ensure that the addition amount of the sodium acetate in the impregnation liquid is 0.05g/L, and then carrying out primary impregnation treatment at the temperature of 85 ℃ for 2 hours; after the primary dipping treatment is finished, filtering solid substances to obtain primary cold alkali dipping waste liquid;
(2) Adding 10g of lithium chloride into the primary cold alkali impregnation waste liquid obtained in the step (1) to obtain a mixed solution A;
(3) Stirring the mixed solution A obtained in the step (1) at 85 ℃ for reacting for 60min to obtain a mixture system;
(4) And (4) dropwise adding 100mL of 0.1 g/mL polyaluminum chloride into the mixture obtained in the step (3) under the condition of stirring, wherein the stirring speed is 2000-4000 rpm, the stirring speed is 200-500 rpm after the addition is finished, and carrying out precipitation reaction for 10min.
(5) Performing suction filtration on the mixture system subjected to the precipitation reaction in the step (4), and separating solid from liquid to obtain a primary solid organic sediment and a primary alkaline recovery liquid;
(6) Adding 0.7kg of poplar chips into the alkaline recovery liquid obtained in the step (5), and supplementing a proper amount of caustic soda to ensure that the alkaline concentration in the impregnation liquid is 40g/L, and performing secondary impregnation treatment at the temperature of 60 ℃ for 4 hours; after the secondary impregnation treatment is finished, filtering solid substances to obtain secondary cold alkali impregnation waste liquid; and (4) repeating the operation steps (2) to (5) to obtain a secondary solid organic sediment and a secondary alkaline recovery liquid.
The total hemicellulose and acetyl hemicellulose contents in the primary solid organic precipitate of the examples of the present application were measured, and the measurement results are shown in the following table 3-1:
TABLE 3-1
The contents of main components and pH of the primary cold alkali impregnation waste liquid and the primary alkali recovery liquid in the examples of the present application were measured, and the measurement results are shown in the following tables 3 to 2:
TABLE 3-2
In table 3-2, "-" indicates that no corresponding component was detected, and it can be seen from table 3-2 that the treatment method of the embodiment of the present application can precipitate more than 80% of the organic matters in the primary cold alkali impregnation waste liquid, i.e. can efficiently separate the organic matters from the waste liquid, and the pH of the waste liquid can still maintain a high alkaline level before and after the separation.
Example 4
It is different from example 3 in that 10g of calcium chloride was added in step (2), and the other treatment processes were the same as in example 3.
The total hemicellulose and acetyl hemicellulose contents of the primary solid organic precipitate of the examples of the present application were measured, and the measurement results are shown in the following table 4-1:
TABLE 4-1
The contents of main components and pH of the primary cold alkali impregnation waste liquid and the primary alkali recovery liquid in the examples of the present application were measured, and the measurement results are shown in the following table 4-2:
TABLE 4-2
The "-" in table 4-2 indicates that no corresponding component was detected, and it can be seen from table 4-2 that the treatment method of the embodiment of the present application can precipitate more than 50% of the organic matters in the primary cold alkali-impregnation waste liquid, and the pH of the waste liquid can still maintain a high alkaline level before and after the separation.
Example 5
It is different from example 3 in that 10g of sodium chloride was added in step (2), and the other treatment processes were the same as example 3.
The total hemicellulose and acetyl hemicellulose contents in the primary solid organic precipitate of the examples of the present application were measured, and the measurement results are shown in the following table 5-1:
TABLE 5-1
The contents of main components and the pH of the primary cold alkali impregnation waste liquid and the primary alkali recovery liquid in the examples of the present application were measured, and the measurement results are shown in the following table 5-2:
TABLE 5-2
In Table 5-2, "-" indicates that no corresponding component was detected, and it can be seen from Table 5-2 that the treatment method of the embodiment of the present application can precipitate more than 30% of the organic substances in the primary cold alkali impregnation waste liquid, and the pH of the waste liquid can still maintain a high alkalinity level before and after the separation.
Examples 3, 4 and 5 show that adding lithium chloride to the alkali impregnation effluent results in better separation results than adding calcium chloride and sodium chloride to the cold alkali impregnation effluent.
Comparative example 1
It is different from example 1 in that sodium acetate is not added in step (1) and other processing techniques are the same as example 1.
The total hemicellulose and acetyl hemicellulose contents of the primary solid organic precipitates of the examples of the present application were measured, and the measurement results are shown in table 6 below:
TABLE 6
Example 1 compared to comparative example 1 shows that the addition of sodium acetate in step (1) is effective in increasing the acetyl hemicellulose content of the primary solid organic sediment.
According to the embodiment of the application, acetate is added in the pulping pretreatment process to form a new acetate-sodium hydroxide buffer system, and the primary alkaline recovery liquid obtained by separating solid organic matters is subjected to secondary circulation pulping, so that the pulping pretreatment process promotes the dissolution of hemicellulose and obtains acetyl hemicellulose with high application value.
The above examples only express several embodiments of the present application, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present application. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the concept of the present application, which falls within the scope of protection of the present application. Therefore, the protection scope of the present patent application shall be subject to the appended claims.
Claims (10)
1. A pretreatment process of paper pulp production raw materials is characterized by comprising the following steps:
adding caustic soda into the wood chip raw material to carry out impregnation treatment to obtain cold alkali impregnation waste liquid; soluble acetate is also added in the dipping treatment process;
adding a pretreatment reagent into the cold alkali dipping waste liquid to carry out pretreatment reaction, and obtaining a first mixture system after the pretreatment reaction is finished;
adding a flocculating agent into the first mixture system for precipitation reaction, and obtaining a second mixture system after the precipitation reaction is finished;
carrying out solid-liquid separation on the second mixture system to obtain a solid organic sediment and an alkaline recovery solution;
and recycling the alkaline recovery liquid to be used as the impregnation liquid of the impregnation treatment.
2. The pulp production feedstock pretreatment process of claim 1, wherein the soluble acetate salt is at least one of sodium acetate and potassium acetate.
3. The pretreatment process of a pulp production raw material according to claim 2, wherein in the impregnation treatment, the mass ratio of the wood chip raw material to the caustic soda is 1:2 to 1:10; the addition amount of the acetate is 0.01-10 g/L.
4. A pulp production feedstock pretreatment process as claimed in claim 1, wherein said pretreatment agent is at least one of a hydrophobic modifier, a free radical reaction initiator, and a metal ion salting-out agent.
5. The pulp production feedstock pretreatment process of claim 4, wherein the hydrophobic modifier is at least one of a silane coupling agent, a 1, 2-alkylene oxide, an alkenyl succinic anhydride; and/or
The free radical reaction initiator is at least one of persulfate, azo compounds and hydroperoxide; and/or
The metal ion salting-out agent is at least one of sodium chloride, potassium chloride and lithium chloride.
6. The pulp production raw material pretreatment process of claim 5, wherein the silane coupling agent is at least one of gamma-chloropropyltriethoxysilane, gamma-chloropropylmethyldichlorosilane, gamma-chloropropyltrimethoxysilane, gamma-aminopropyltriethoxysilane, gamma-aminopropyltrimethoxysilane; and/or
The persulfate is at least one of potassium persulfate, sodium persulfate and ammonium persulfate.
7. The pulp production feedstock pretreatment process of claim 1, wherein the flocculant is at least one of polyaluminum chloride, cationic polyacrylamide, ferric chloride.
8. The pulp production raw material pretreatment process according to any one of claims 1 to 7, wherein the amount of the hydrophobic modifier added is 10 to 20g/L; and/or
The adding amount of the free radical reaction initiator is 5-15 g/L; and/or
The dosage of the metal ion salting-out agent is 5-15 g/L.
9. The pulp production feedstock pretreatment process of claim 8, wherein the flocculant is added in an amount of 0.1 to 0.4g/L.
10. A process for pretreating pulp production raw material according to any of claims 1 to 7, wherein the impregnation is carried out at a temperature of 20 to 90 ℃ for 2 to 6 hours.
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| WO2024040677A1 (en) * | 2022-08-23 | 2024-02-29 | 天津科技大学 | Chemical alkali recovery treatment process for chemimechanical pulping waste liquid |
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