CN109403115A - A method of vinegar-grade dissolving pulp is produced using poplar slab - Google Patents
A method of vinegar-grade dissolving pulp is produced using poplar slab Download PDFInfo
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- CN109403115A CN109403115A CN201811228170.XA CN201811228170A CN109403115A CN 109403115 A CN109403115 A CN 109403115A CN 201811228170 A CN201811228170 A CN 201811228170A CN 109403115 A CN109403115 A CN 109403115A
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- 241000219000 Populus Species 0.000 title claims abstract description 46
- 229920000875 Dissolving pulp Polymers 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims description 45
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 23
- 238000004061 bleaching Methods 0.000 claims abstract description 21
- 230000007062 hydrolysis Effects 0.000 claims abstract description 10
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- 239000000654 additive Substances 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- 239000012752 auxiliary agent Substances 0.000 claims description 24
- 239000002002 slurry Substances 0.000 claims description 22
- 230000008569 process Effects 0.000 claims description 21
- 102000004190 Enzymes Human genes 0.000 claims description 20
- 108090000790 Enzymes Proteins 0.000 claims description 20
- 238000009835 boiling Methods 0.000 claims description 20
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 18
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 12
- 239000003513 alkali Substances 0.000 claims description 12
- 238000002791 soaking Methods 0.000 claims description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 11
- 230000035484 reaction time Effects 0.000 claims description 10
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 9
- 235000010265 sodium sulphite Nutrition 0.000 claims description 9
- 229920002678 cellulose Polymers 0.000 claims description 8
- 239000001913 cellulose Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 8
- 239000000347 magnesium hydroxide Substances 0.000 claims description 8
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 238000000605 extraction Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 4
- 229920002472 Starch Polymers 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 239000001814 pectin Substances 0.000 claims description 4
- 229920001277 pectin Polymers 0.000 claims description 4
- 235000010987 pectin Nutrition 0.000 claims description 4
- -1 polyoxyethylene Polymers 0.000 claims description 4
- UKLNMMHNWFDKNT-UHFFFAOYSA-M sodium chlorite Chemical compound [Na+].[O-]Cl=O UKLNMMHNWFDKNT-UHFFFAOYSA-M 0.000 claims description 4
- 229960002218 sodium chlorite Drugs 0.000 claims description 4
- 235000019698 starch Nutrition 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 3
- 108010064470 polyaspartate Proteins 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- PQHYOGIRXOKOEJ-UHFFFAOYSA-N 2-(1,2-dicarboxyethylamino)butanedioic acid Chemical compound OC(=O)CC(C(O)=O)NC(C(O)=O)CC(O)=O PQHYOGIRXOKOEJ-UHFFFAOYSA-N 0.000 claims description 2
- 241000432824 Asparagus densiflorus Species 0.000 claims description 2
- 239000002028 Biomass Substances 0.000 claims description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- WUFSRLQSIDFFMT-UHFFFAOYSA-N oxirane;phosphoric acid Chemical compound C1CO1.OP(O)(O)=O WUFSRLQSIDFFMT-UHFFFAOYSA-N 0.000 claims description 2
- 238000010411 cooking Methods 0.000 abstract description 6
- 238000012545 processing Methods 0.000 abstract description 5
- 239000002023 wood Substances 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 230000002255 enzymatic effect Effects 0.000 abstract 1
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 17
- 239000002994 raw material Substances 0.000 description 11
- 229920002488 Hemicellulose Polymers 0.000 description 10
- 239000002956 ash Substances 0.000 description 8
- 238000006116 polymerization reaction Methods 0.000 description 8
- 230000004044 response Effects 0.000 description 8
- 238000005516 engineering process Methods 0.000 description 7
- 229920002301 cellulose acetate Polymers 0.000 description 6
- 150000002972 pentoses Chemical class 0.000 description 6
- 235000002918 Fraxinus excelsior Nutrition 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 229920005610 lignin Polymers 0.000 description 4
- 230000009257 reactivity Effects 0.000 description 4
- BAZVSMNPJJMILC-UHFFFAOYSA-N triadimenol Chemical compound C1=NC=NN1C(C(O)C(C)(C)C)OC1=CC=C(Cl)C=C1 BAZVSMNPJJMILC-UHFFFAOYSA-N 0.000 description 4
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 3
- 229920001747 Cellulose diacetate Polymers 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 238000006467 substitution reaction Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- QMMFVYPAHWMCMS-UHFFFAOYSA-N Dimethyl sulfide Chemical compound CSC QMMFVYPAHWMCMS-UHFFFAOYSA-N 0.000 description 1
- 244000166124 Eucalyptus globulus Species 0.000 description 1
- 240000007472 Leucaena leucocephala Species 0.000 description 1
- 235000010643 Leucaena leucocephala Nutrition 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 229920000805 Polyaspartic acid Polymers 0.000 description 1
- 206010036590 Premature baby Diseases 0.000 description 1
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 1
- 230000021736 acetylation Effects 0.000 description 1
- 238000006640 acetylation reaction Methods 0.000 description 1
- 238000005903 acid hydrolysis reaction Methods 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 210000000630 fibrocyte Anatomy 0.000 description 1
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 description 1
- 238000009897 hydrogen peroxide bleaching Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 125000001841 imino group Chemical group [H]N=* 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000004076 pulp bleaching Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 108091008146 restriction endonucleases Proteins 0.000 description 1
- 238000001223 reverse osmosis Methods 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 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
- D21C3/00—Pulping cellulose-containing materials
- D21C3/02—Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes
- D21C3/022—Pulping cellulose-containing materials with inorganic bases or alkaline reacting compounds, e.g. sulfate processes in presence of S-containing 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
- D21C3/00—Pulping cellulose-containing materials
- D21C3/22—Other features of pulping processes
-
- 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
- D21C1/02—Pretreatment of the finely-divided materials before digesting with water or steam
-
- 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
- D21C3/00—Pulping cellulose-containing materials
- D21C3/003—Pulping cellulose-containing materials with organic 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
- D21C3/00—Pulping cellulose-containing materials
- D21C3/006—Pulping cellulose-containing materials with compounds not otherwise provided for
-
- 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
- D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
- D21C5/005—Treatment of cellulose-containing material with microorganisms or enzymes
-
- 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
- D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
- D21C9/10—Bleaching ; Apparatus therefor
-
- 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
- D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
- D21C9/10—Bleaching ; Apparatus therefor
- D21C9/1005—Pretreatment of the pulp, e.g. degassing the pulp
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- Microbiology (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Inorganic Chemistry (AREA)
- Paper (AREA)
Abstract
本发明涉及溶解浆制备技术领域，特别涉及一种利用杨木板皮生产醋化级溶解浆的方法：添加助剂预水解；Soda/AQ蒸煮Ⅰ段；Soda/AQ蒸煮Ⅱ段；OPDQEPP漂白；酶协同处理。制备了高纯度和高反应活性的杨木板皮醋化级溶解浆；所用化学品清洁环保，生产工艺清洁。
The invention relates to the technical field of dissolving pulp preparation, in particular to a method for producing vinegar-grade dissolving pulp by using poplar wood veneer: pre-hydrolysis with additives; Soda/AQ cooking stage I; Soda/AQ cooking stage II; O P D Q E PP bleaching; enzymatic co-processing. High-purity and high-reactivity poplar board veneer vinegar-grade dissolving pulp is prepared; the chemicals used are clean and environmentally friendly, and the production process is clean.
Description
Technical field
The present invention relates to dissolving pulp preparation technical fields, in particular to a kind of to produce vinegar-grade dissolving pulp using poplar slab
Method.
Background technique
Currently, nearly 1,000,000 tons of cellulose acetate yield in the world, and China produces nearly 400,000 tons of cellulose acetate per year, year consumes vinegar-grade
About 300,000 tons of the wooden dissolving pulp, vinegar-grade dissolving pulp is mainly used to prepare Triafol T and cellulose diacetate, in dissolving pulp
Hydroxyl almost acetylation on cellulose glucose unit on 2,3,6 three positions, obtaining Triafol T, (degree of substitution is
> 2.7), Triafol T hydrolyzes to obtain cellulose diacetate (degree of substitution 2.4-2.6), and reaction process is shown below.
Triafol T is widely used in film, liquid crystal display polarizing coating, reverse osmosis membrane etc., and cellulose diacetate is wide
It is general to apply to cigaratte filter, plastic products etc..Cellulose acetate has higher requirement to its raw material-vinegar-grade dissolving pulp, i.e., high
Purity and high reaction activity, currently, China can only prepare vinegar-grade Cotton Pulp, and the vinegar-grade of high-purity, high reaction activity
The wooden dissolving pulp relies primarily on import.
Be both at home and abroad that raw material prepare vinegar-grade dissolving pulp using timber, technique generally use prehydrolysis+sulphate cook+
ECF bleaching process or acid accumulator sulfite boiling+ECF bleaching+cold alkali density technique, in order to improve going for prehydrolysis hemicellulose
Except rate, inorganic acid or organic acid are usually added, which increase the corrosivity of equipment.In order to improve delignification rate, some researchers
Using the KP method boiling technology of high curing degree, but high sulphidity is also easy to produce the foul smell such as methyl mercaptan, dimethyl sulphide；It is molten in order to reduce
The ash content of slurry is solved, dissolving pulp manufacturing enterprise will carry out sour processing after paper pulp bleaching, but low pH value easily makes part in dissolving pulp
Cellulose occurs acidic hydrolysis and drops poly-；In order to improve the alpha-cellulose content of vinegar-grade dissolving pulp, some scholars use cold alkali
Extracting, but this can seriously reduce the reactivity ability of vinegar-grade dissolving pulp and aceticanhydride, some Egyptian scholar's microwave radiations and
Highly concentrated zinc chloride handles vinegar-grade dissolving pulp to improve its reactivity, but technology also prematurity；United States Patent (USP) report
Its purity is improved using strong acid treatment vinegar-grade dissolving pulp, but this technology pollution level is high, it is at high cost.Domestic Ye Youjisuo universities and colleges
The positive research and development for carrying out this respect technology, mainly there is the units such as South China Science & Engineering University, Beijing Forestry University and Donghua University
It is had made some progress in the research and development of the technology, is concentrated mainly on Eucalyptus, Acacia, pine and prepares vinegar-grade dissolution
Slurry.
Poplar slab is cheap, raw material is sufficient as wood machining residues, it is reported that, the annual timber processing in China is surplus
About 50,000,000 tons of the yield of excess, the one kind of poplar slab as wood machining residues, holocellulose content is about 82%,
Wherein alpha-cellulose content is about 44%, will be to acetifying if producing high reaction activity vinegar-grade dissolving pulp by raw material of poplar slab
The exploitation of grade dissolving pulp raw material is of great advantage.But both at home and abroad without the record for using poplar slab to prepare vinegar-grade dissolving pulp.
Summary of the invention
It is above in the prior art without the technological gap for using poplar slab to prepare vinegar-grade dissolving pulp, the application in order to solve
Disclose a kind of method using poplar slab production vinegar-grade dissolving pulp.
It is selectively protected while hemicellulose in removing poplar slab raw material using the prehydrolysis technology of addition auxiliary agent
Cellulose, and swollen fibrocyte are protected, then uses stage cooking, selectively removing lignin and hemicellulose, controls cellulose
Drop is poly-, and slurry carries out hydrogen peroxide reinforced-oxygen bleaching/addition chelating agent ClO 2 bleaching/addition hydrogen peroxide after boiling
Hot alkali extraction/hydrogen peroxide bleaching (OPDQEPP remaining lignin and hemicellulose) are removed, pulp brightness is improved and adjusts dissolution
The degree of polymerization of slurry, to after drift slurry carry out biological enzyme collaboration processing further increase its acetify response value (PV value), reduce ash content and
Methylene chloride (DCM) the extractives content.After this process, the purity and reactivity of vinegar-grade dissolving pulp are improved.
What the present invention was obtained through the following steps:
A method of vinegar-grade dissolving pulp is produced using poplar slab, comprising the following steps:
(1) add auxiliary agent prehydrolysis: liquor ratio 1:(4~10), hydrolysis additive dosage be poplar slab dry biomass 0.1~
2.0%, 80~170 DEG C of hydrolysis temperature, soaking time 10~180 minutes, hydrolysis auxiliary agent was Boratex, magnesium sulfate, polyoxyethylene nonyl phenyl
The mixture that ethylene ether phosphate and four sodium of iminodisuccinic acid are mixed to get according to mass ratio 1:1:1:1；
(2) I section of Soda/AQ boiling；
(3) II section of Soda/AQ boiling；
(4) OPDQEPP bleaching；
(5) enzyme collaboration is handled: slurry dense 2~10%, 30-50 DEG C of temperature, handles time 60min, pH=4.0~7.0, poly- asparagus fern ammonia
Sour dosage is the 0.01%-1.0% of oven dry stock quality, and OP-13 dosage is the 0.001-0.01% of oven dry stock quality, OP-15 dosage
For the 0.001-0.01% of oven dry stock quality, cellulose inscribe enzyme dosage is 0.1~0.6IU/gpulp, and zytase dosage is 2
~4XU/gpulp, pectin enzyme dosage are 0.1~10 IU/gpulp.
It is preferred that I segment process condition of Soda/AQ boiling are as follows: with Na2O counts 5~15% that alkali charge is oven dry stock quality, liquor ratio
1:(3~8), magnesium hydroxide dosage be oven dry stock quality 0.5%, sodium sulfite dosage be oven dry stock quality 1.0~
10.0%, AQ dosage be oven dry stock quality 0.05%, 80~120 DEG C of temperature, soaking time 10~180 minutes.
It is preferred that II segment process condition of Soda/AQ boiling are as follows: with Na2O counts 5~25% that alkali charge is oven dry stock quality, hydrogen-oxygen
Change 0.5% that magnesium dosage is oven dry stock quality, sodium sulfite dosage is the 1.0~10.0% of oven dry stock quality, liquor ratio 1:(3~
10), AQ dosage be oven dry stock quality 0.05%, 140~180 DEG C of temperature, soaking time 10~240 minutes.
It is preferred that OPDQEPP bleaching conditions are as follows: OPThe oxygen pressure of drift is 0.4~0.6Mpa, starches dense 10%, MgSO4Dosage is
0.6%, the NaOH dosage of oven dry stock quality is 1.0~3.0%, H of oven dry stock quality2O2Dosage be oven dry stock quality 0.5~
3.0%, 70~110 DEG C of temperature, keep the temperature 60min..
It is preferred that OPDQEPP bleaching conditions are as follows: QD10~120 minutes reaction time of bleaching process, T=30 ± 2 DEG C, slurry
Dense 2~8%, pH=1~3, sodium chlorite dosage are the 0.2-6.0% of oven dry stock quality, and IDS dosage is the 0.01 of oven dry stock quality
~1.0%.
It is preferred that OPDQEPP bleaching conditions are as follows: the 30~180min. of reaction time, MgSO of Ep extraction process4Dosage is
0.5%, the NaOH dosage of oven dry stock quality is the 0.5-5.0%, H of oven dry stock quality2O2Dosage is the 1.0- of oven dry stock quality
5.0%, IDS dosage are the 0.01~1.0% of oven dry stock quality, slurry dense 8%, 70~95 DEG C of temperature.
It is preferred that OPDQEPP bleaching conditions are as follows: the 60~180min. of reaction time, MgSO of P drift4Dosage is oven dry stock
0.5%, the NaOH dosage of quality is that 0.4%, the NaAC dosage of oven dry stock quality is 0.4%, H of oven dry stock quality2O2Dosage is
The 1.0-5.0% of oven dry stock quality, slurry dense 10%, 80~95 DEG C of temperature.
In conclusion by adding auxiliary agent in poplar slab prehydrolysis come the hemicellulose in selectively removing poplar slab,
Then using the Soda/AQ stage cooking of addition auxiliary agent, as far as possible removing lignin, cellulose is protected, slurry carries out after boiling
OPDQEPP bleaching further removes lignin and adjusts the degree of polymerization of dissolving pulp, finally, with enzyme collaboration technique to the purity of dissolving pulp
The reactivity for further increasing and adjusting dissolving pulp obtains the poplar slab vinegar-grade dissolution of high-purity and high reaction activity
Slurry.
Beneficial effects of the present invention:
(1) hemicellulose in poplar slab is significantly selectively dissolved out by means of the prehydrolysis of addition auxiliary agent first, is finally adopted
Take enzyme collaboration processing to further increase the purity of poplar slab slurry and acetify response value, in conjunction with Soda/AQ stage cooking and
OPDQEPP bleaching, is prepared for the poplar slab vinegar-grade dissolving pulp of high-purity and high reaction activity；
(2) process poplar slab of the present invention, chemicals clean and environmental protection used, production technology cleaning are used.
Detailed description of the invention
Fig. 1 is the process flow chart that poplar slab produces vinegar-grade dissolving pulp.
Specific embodiment
In order to better understand the present invention, it is further illustrated below with reference to specific example.
It is Boratex, magnesium sulfate, thermally coupled distillation columns and imino group that auxiliary agent is hydrolyzed in following embodiment
The mixture that four sodium of disuccinic acid is mixed to get according to mass ratio 1:1:1:1.
The percentage composition of material used is its percentage composition for accounting for oven dry stock quality in each operation stage.
Embodiment 1:
Add prehydrolysis-addition auxiliary agent Soda/AQ stage cooking-O of auxiliary agentPQDEpP- enzyme cooperates with process poplar slab
Raw material: taking the poplar slab piece of 500g factory, long 10-30mm, hemi-cellulose content 24.3%, and alpha-cellulose content is
43.0%。
The pre-hydrolysis technique condition of control addition auxiliary agent are as follows: liquor ratio 1:6, auxiliary agent 0.4%, 160 DEG C of maximum temperature, when heat preservation
Between 60 minutes, after hydrolysis hemi-cellulose content be 8.6%, hydrolyze yield 80%；
I segment process condition of Soda/AQ boiling are as follows: alkali charge 5%, liquor ratio 1:4, magnesium hydroxide 0.5%, sodium sulfite are
5.0%, AQ dosage be 0.05%, Tmax=100 DEG C ± 2 DEG C, soaking time 60 minutes；
II segment process condition of Soda/AQ boiling are as follows: alkali charge 18%, magnesium hydroxide 0.5%, sodium sulfite are 3.0 %, liquor ratio
1:7, AQ dosage be 0.05%, 160 DEG C of maximum temperature, soaking time 120 minutes；
OPThe oxygen pressure of drift is 0.5Mpa, starches dense 10%, MgSO40.6%, NaOH 2.0%, H2O21.0%, 95 DEG C of temperature, heat preservation
60min；
QDDense 4.0%, pH=1.5, sodium chlorite dosage 3.0%, IDS are starched in the 60 minutes reaction time of bleaching process, T=30 ± 2 DEG C
Dosage 0.05%；
The reaction time 90min., MgSO of Ep extraction process40.5%, NaOH 3.0%, H2O22.0%, IDS dosage 0.05%, slurry
Dense 8%, 85 DEG C of temperature；
The reaction time 120min., MgSO of P drift40.5%, NaOH 0.4%, NaAC 0.4%, H2O23.0%, slurry dense 10%, temperature
90 DEG C of degree；
Enzyme cooperates with treatment conditions are as follows: slurry dense 5%, handles time 60min, pH=5.0, poly-aspartate by 40 DEG C of temperature
(polyaspartic acid) dosage 0.05%, OP-13 dosage 0.005%, OP-15 dosage 0.005%, cellulose restriction endonuclease
Dosage is 0.2IU/gpulp, and zytase dosage is 3XU/gpulp, and pectin enzyme dosage is 3 IU/gpulp.
The alpha-cellulose content for obtaining poplar slab vinegar-grade dissolving pulp is 97%, poly-pentose 2.6%, the degree of polymerization 1250,
Whiteness 89%ISO, content of ashes 0.01%, DCM the extractives content 0.03% acetify response value (PV value) 800.
Every Testing index of poplar slab vinegar-grade dissolving pulp is preferable, can be used to produce high-grade cellulose acetate production
Product.
Embodiment 2:
Add prehydrolysis-addition auxiliary agent Soda/AQ stage cooking-O of auxiliary agentPQDEpP- enzyme cooperates with process poplar slab
Raw material, the hemi-cellulose content of taken poplar slab are 22.3%, alpha-cellulose content 45.0%, process conditions with embodiment 1
It is identical.The alpha-cellulose content for obtaining poplar slab vinegar-grade dissolving pulp is 97%, poly-pentose 2.2%, and the degree of polymerization 1280 is white
90%ISO, content of ashes 0.01% are spent, DCM the extractives content 0.02% acetifies response value (PV value) 820.
Every Testing index of poplar slab vinegar-grade dissolving pulp is preferable, can be used to produce high-grade cellulose acetate production
Product.
Embodiment 3:
Add prehydrolysis-addition auxiliary agent Soda/AQ stage cooking-O of auxiliary agentPQDEpP- enzyme cooperates with process poplar slab
Raw material, taken poplar slab is the same as embodiment 1.Only changing prehydrolysis soaking time is 120 minutes, and hemi-cellulose content is after hydrolysis
8.5%, yield 79% is hydrolyzed, other techniques are constant.The alpha-cellulose content for finally obtaining poplar slab vinegar-grade dissolving pulp is
97%, poly-pentose 2.2%, the degree of polymerization 1200, whiteness 89%ISO, content of ashes 0.01%, DCM the extractives content 0.02% acetifies
Response value (PV value) 780.
Embodiment 4:
Add prehydrolysis-addition auxiliary agent Soda/AQ stage cooking-O of auxiliary agentPQDEpP- enzyme cooperates with process poplar slab
Raw material, taken poplar slab is the same as embodiment 1.Only changing II section of cooking liquor ratio of Soda/AQ boiling is 1:4, other techniques are constant.Most
The alpha-cellulose content for obtaining poplar slab vinegar-grade dissolving pulp eventually is 97%, poly-pentose 2.5%, the degree of polymerization 1060, whiteness
90%ISO, content of ashes 0.01%, DCM the extractives content 0.02% acetify response value (PV value) 730.
Every Testing index of poplar slab vinegar-grade dissolving pulp is preferable, can be used to produce high-grade cellulose acetate production
Product.
Embodiment 5:
Add the Soda/AQ stage cooking-O of auxiliary agentPQDEpP- enzyme cooperates with process poplar slab raw material, taken poplar slab
With embodiment 1.Step addition auxiliary agent prehydrolysis is removed, liquor ratio 1:6, other techniques are identical with embodiment 1.Finally obtain poplar
The alpha-cellulose content of plank skin vinegar-grade dissolving pulp is 95%, poly-pentose 3.6%, the degree of polymerization 1200, whiteness 88%ISO, ash
Divide content 0.015%, DCM the extractives content 0.025% acetifies response value (PV value) 680.
Embodiment 6:
Add prehydrolysis-addition auxiliary agent Soda/AQ stage cooking-O of auxiliary agentPQDEpP- enzyme cooperates with process poplar slab
Raw material, taken poplar slab is the same as embodiment 1.One section of boiling is merged into two sections of boilings of step (2) and (3), two sections of boilings are used
Alkali, magnesium hydroxide, sodium sulfite, AQ are added at one time, liquor ratio 1:6, Tmax=100 DEG C ± 2 DEG C, and soaking time 60 minutes；Then
160 DEG C keep the temperature 120 minutes, other techniques are identical with embodiment 1.Finally obtain the alpha-cellulose of poplar slab vinegar-grade dissolving pulp
Content is 96%, poly-pentose 2.7%, the degree of polymerization 1000, whiteness 89%ISO, content of ashes 0.01%, DCM the extractives content
0.02%, acetify response value (PV value) 700.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by the limit of embodiment
System, other any changes made without departing from the spirit and principles of the present invention, modification, combination, substitution, simplification should be
Equivalence replacement mode, is included within the scope of the present invention.
Claims (9)
1. a kind of method using poplar slab production vinegar-grade dissolving pulp, it is characterised in that the following steps are included:
(1) add auxiliary agent prehydrolysis: liquor ratio 1:(4~10), hydrolysis additive dosage be poplar slab dry biomass 0.1~
2.0%, 80~170 DEG C of hydrolysis temperature, soaking time 10~180 minutes, hydrolysis auxiliary agent was Boratex, magnesium sulfate, polyoxyethylene nonyl phenyl
The mixture that ethylene ether phosphate and four sodium of iminodisuccinic acid are mixed to get according to mass ratio 1:1:1:1；
(2) I section of Soda/AQ boiling；
(3) II section of Soda/AQ boiling；
(4) OPDQEPP bleaching；
(5) enzyme collaboration is handled: slurry dense 2~10%, 30-50 DEG C of temperature, handles time 60min, pH=4.0~7.0, poly- asparagus fern ammonia
Sour dosage is the 0.01%-1.0% of oven dry stock quality, and OP-13 dosage is the 0.001-0.01% of oven dry stock quality, OP-15 dosage
For the 0.001-0.01% of oven dry stock quality, cellulose inscribe enzyme dosage is 0.1~0.6IU/gpulp, and zytase dosage is 2
~4XU/gpulp, pectin enzyme dosage are 0.1~10 IU/gpulp.
2. according to the method described in claim 1, it is characterized in that I segment process condition of Soda/AQ boiling are as follows: with Na2O meter uses alkali
Amount is the 5~15% of oven dry stock quality, liquor ratio 1:(3~8), magnesium hydroxide dosage is the 0.5% of oven dry stock quality, sodium sulfite
Dosage is that 1.0~10.0%, the AQ dosage of oven dry stock quality is the 0.05% of oven dry stock quality, 80~120 DEG C of temperature, soaking time
10~180 minutes.
3. according to the method described in claim 1, it is characterized in that II segment process condition of Soda/AQ boiling are as follows: with Na2O meter uses alkali
Amount is the 5~25% of oven dry stock quality, and magnesium hydroxide dosage is the 0.5% of oven dry stock quality, and sodium sulfite dosage is oven dry stock matter
The 1.0~10.0% of amount, liquor ratio 1:(3~10), AQ dosage is the 0.05% of oven dry stock quality, 140~180 DEG C of temperature, when heat preservation
Between 10~240 minutes.
4. according to the method described in claim 1, it is characterized in that OPDQEPP bleaching conditions are as follows: OPThe oxygen pressure of drift is 0.4
~0.6Mpa starches dense 10%, MgSO4Dosage is that 0.6%, the NaOH dosage of oven dry stock quality is the 1.0~3.0% of oven dry stock quality,
H2O2Dosage is the 0.5~3.0% of oven dry stock quality, 70~110 DEG C of temperature, keeps the temperature 60min..
5. according to the method described in claim 1, it is characterized in that OPDQEPP bleaching conditions are as follows: QDThe reaction of bleaching process
Time 10~120 minutes, dense 2~8%, pH=1~3 were starched in T=30 ± 2 DEG C, and sodium chlorite dosage is the 0.2- of oven dry stock quality
6.0%, IDS dosage are the 0.01~1.0% of oven dry stock quality.
6. according to the method described in claim 1, it is characterized in that OPDQEPP bleaching conditions are as follows: the reaction of Ep extraction process
30~180min. of time, MgSO4Dosage is that 0.5%, the NaOH dosage of oven dry stock quality is the 0.5-5.0% of oven dry stock quality
, H2O2Dosage is the 1.0-5.0% of oven dry stock quality, and IDS dosage is the 0.01~1.0% of oven dry stock quality, slurry dense 8%, temperature 70
~95 DEG C.
7. according to the method described in claim 1, it is characterized in that OPDQEPP bleaching conditions are as follows: the reaction time 60 of P drift
~180min., MgSO4Dosage is that 0.5%, the NaOH dosage of oven dry stock quality is 0.4%, the NaAC dosage of oven dry stock quality
For 0.4%, H of oven dry stock quality2O21.0-5.0% of the dosage for oven dry stock quality, slurry dense 10%, 80~95 DEG C of temperature.
8. according to the method described in claim 1, characterized by the following steps:
(1) add auxiliary agent prehydrolysis: liquor ratio 1:6, auxiliary dosage be oven dry stock quality 0.4%, 160 DEG C of temperature, soaking time
60 minutes；
(2) I section of Soda/AQ boiling: alkali charge is the 5% of oven dry stock quality, and liquor ratio 1:4, magnesium hydroxide dosage is oven dry stock matter
The 0.5% of amount, sodium sulfite dosage is that 5.0%, the AQ dosage of oven dry stock quality is 0.05%, Tmax=100 of oven dry stock quality
DEG C ± 2 DEG C, soaking time 60 minutes；
(3) II section of Soda/AQ boiling: alkali charge is the 18% of oven dry stock quality, and magnesium hydroxide dosage is oven dry stock quality
0.5%, sodium sulfite dosage is 3.0 % of oven dry stock quality, and liquor ratio 1:7, AQ dosage is the 0.05% of oven dry stock quality, highest
160 DEG C of temperature, soaking time 120 minutes；
(4) OPDQEPP bleaches OPThe oxygen pressure of drift is 0.5Mpa, starches dense 10%, MgSO4Dosage is that 0.6%, NaOH of oven dry stock quality is used
Amount is 2.0%, H of oven dry stock quality2O2Dosage is the 1.0% of oven dry stock quality, 95 DEG C of temperature, keeps the temperature 60min；QDBleaching process
Reaction time 60 minutes, dense 4.0%, pH=1.5 are starched in T=30 ± 2 DEG C, and sodium chlorite dosage is 3.0%, IDS of oven dry stock quality
Dosage is the 0.05% of oven dry stock quality；The reaction time 90min., MgSO of Ep extraction process4Dosage is oven dry stock quality
0.5%, NaOH dosage are 3.0%, H of oven dry stock quality2O2Dosage is that 2.0%, the IDS dosage of oven dry stock quality is oven dry stock matter
The 0.05% of amount, slurry dense 8%, 85 DEG C of temperature；The reaction time 120min., MgSO of P drift4Dosage is the 0.5% of oven dry stock quality,
NaOH dosage is that 0.4%, the NaAC dosage of oven dry stock quality is 0.4%, H of oven dry stock quality2O2Dosage is oven dry stock quality
3.0%, slurry dense 10%, 90 DEG C of temperature；
(5) enzyme collaboration is handled: slurry dense 5%, 40 DEG C of temperature, handles time 60min, pH=5.0, poly-aspartate dosage is over dry
0.05%, the OP-13 dosage of slurry quality is that 0.005%, the OP-15 dosage of oven dry stock quality is the 0.005% of oven dry stock quality, fine
Tieing up plain inscribe enzyme dosage is 0.2IU/gpulp, and zytase dosage is 3XU/gpulp, and pectin enzyme dosage is 3 IU/gpulp.
9. according to the method described in claim 1, it is characterized in that the long 10-30mm of poplar slab used in step (1), poly- penta
Sugared content is 22.3-24.3%, alpha-cellulose content 43.0-45.0%.
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811228170.XA CN109403115B (en) | 2018-10-22 | 2018-10-22 | A kind of method that utilizes poplar wood veneer to produce vinegar grade dissolving pulp |
| PCT/CN2018/114525 WO2020082427A1 (en) | 2018-10-22 | 2018-11-08 | Method for using poplar bark to produce acetylation-grade dissolving pulp |
| US16/314,319 US20200173103A1 (en) | 2018-10-22 | 2018-11-08 | Method for producing acetate grade dissolving pulp from poplar residual slabs |
| BE20195709A BE1026675B1 (en) | 2018-10-22 | 2019-10-17 | PROCESS FOR THE PRODUCTION OF ACETATE QUALITY DISSOLVING PASTE FROM RESIDUAL POPLAR SLABS |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811228170.XA CN109403115B (en) | 2018-10-22 | 2018-10-22 | A kind of method that utilizes poplar wood veneer to produce vinegar grade dissolving pulp |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109403115A true CN109403115A (en) | 2019-03-01 |
| CN109403115B CN109403115B (en) | 2020-12-29 |
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|---|---|---|---|
| CN201811228170.XA Expired - Fee Related CN109403115B (en) | 2018-10-22 | 2018-10-22 | A kind of method that utilizes poplar wood veneer to produce vinegar grade dissolving pulp |
Country Status (4)
| Country | Link |
|---|---|
| US (1) | US20200173103A1 (en) |
| CN (1) | CN109403115B (en) |
| BE (1) | BE1026675B1 (en) |
| WO (1) | WO2020082427A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115075033A (en) * | 2022-05-31 | 2022-09-20 | 中国制浆造纸研究院有限公司 | Method for preparing pulp by prehydrolysis sulfate pulp |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111877047B (en) * | 2020-07-13 | 2023-04-18 | 山东银鹰股份有限公司 | Production process of cotton pulp for spinning-grade cellulose diacetate |
| CN111893787B (en) * | 2020-07-13 | 2022-12-09 | 山东银鹰股份有限公司 | Production process of cotton pulp for plastic-grade cellulose diacetate |
| CN115748290B (en) * | 2022-11-21 | 2023-08-22 | 亚太森博（山东）浆纸有限公司 | Low-whiteness and low-DCM extract bleached sulfate hardwood pulp and preparation method thereof, wood pulp board and preparation method thereof |
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| CN109403115B (en) | 2020-12-29 |
| US20200173103A1 (en) | 2020-06-04 |
| BE1026675B1 (en) | 2020-09-21 |
| BE1026675A1 (en) | 2020-04-30 |
| WO2020082427A1 (en) | 2020-04-30 |
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