CN113023996A - Recycling method of squeezed waste alkali liquor generated in viscose production - Google Patents
Recycling method of squeezed waste alkali liquor generated in viscose production Download PDFInfo
- Publication number
- CN113023996A CN113023996A CN202110377458.9A CN202110377458A CN113023996A CN 113023996 A CN113023996 A CN 113023996A CN 202110377458 A CN202110377458 A CN 202110377458A CN 113023996 A CN113023996 A CN 113023996A
- Authority
- CN
- China
- Prior art keywords
- alkali liquor
- hemicellulose
- viscose
- waste alkali
- waste
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- 239000003513 alkali Substances 0.000 title claims abstract description 44
- 239000002699 waste material Substances 0.000 title claims abstract description 32
- 229920000297 Rayon Polymers 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000004064 recycling Methods 0.000 title claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 51
- 229920002488 Hemicellulose Polymers 0.000 claims abstract description 40
- 235000011121 sodium hydroxide Nutrition 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 238000000926 separation method Methods 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 9
- 238000007380 fibre production Methods 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000012716 precipitator Substances 0.000 claims description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 238000001556 precipitation Methods 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 238000013329 compounding Methods 0.000 claims description 5
- 239000006228 supernatant Substances 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 4
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 4
- 239000008394 flocculating agent Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229920002401 polyacrylamide Polymers 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 235000011124 aluminium ammonium sulphate Nutrition 0.000 claims description 2
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 2
- LCQXXBOSCBRNNT-UHFFFAOYSA-K ammonium aluminium sulfate Chemical compound [NH4+].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O LCQXXBOSCBRNNT-UHFFFAOYSA-K 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- 239000012046 mixed solvent Substances 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 239000013557 residual solvent Substances 0.000 claims description 2
- 239000000835 fiber Substances 0.000 abstract description 8
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 238000011084 recovery Methods 0.000 abstract description 4
- 239000006227 byproduct Substances 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000004134 energy conservation Methods 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 abstract 2
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 abstract 2
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 abstract 1
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000012528 membrane Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000000502 dialysis Methods 0.000 description 2
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 description 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- -1 compound polysaccharide Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 125000001483 monosaccharide substituent group Chemical group 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Artificial Filaments (AREA)
Abstract
The invention belongs to the field of resource recycling, relates to a waste alkali liquor waste utilization method, and particularly relates to a waste alkali liquor recycling method in the viscose fiber production process of a chemical fiber plant. According to the method, the hemicellulose is separated from the waste alkali liquor through the reaction unit, the solid-liquid separation unit, the rectification unit, the solid drying unit and the liquid recovery unit, so that the waste alkali liquor can be completely recovered and recycled, meanwhile, a byproduct hemicellulose can be obtained, the hemicellulose can be used as a raw material for producing furfural or xylose, and the added value of waste liquor treatment is increased. Not only is beneficial to energy conservation and emission reduction and environmental pollution reduction, but also can save a large amount of caustic soda, and is very beneficial to environmental protection.
Description
Technical Field
The invention belongs to resource recycling, and particularly relates to a method for recycling waste alkali liquor in the production process of viscose fibers in a chemical fiber plant.
Background
Viscose is one of the main chemical fiber varieties, and the yield of the viscose accounts for about one third of the total global chemical fiber yield. It is estimated that the viscose fiber production capacity in China is about 300 ten thousand tons, and the annual output of the viscose fiber accounts for about 60 percent of the total world output. The amount of viscose fiber used continues to increase with the development of global economy and the growth of the population. The viscose fiber production process comprises 4 stages of viscose preparation, spinning, post-treatment and post-processing, wherein a large amount of caustic soda is consumed in the viscose preparation process, a large amount of waste alkali liquor is generated, the main components of the waste alkali liquor are water, NaOH and hemicellulose, and the content of the NaOH is up to 17-20%. In the viscose fiber production process, the alkali liquor is recycled, but when the concentration of hemicellulose in the alkali liquor is increased to a certain degree, the alkali liquor can not be used for production, otherwise, the viscose preparation process, the viscose property, the forming condition and the quality of a final product can be influenced. In order to control the content of hemicellulose in the alkali liquor, the original method is to adjust the content of hemicellulose in the alkali liquor by partially discharging waste alkali liquor, so that a large amount of acid needs to be consumed for neutralization, the running cost of a sewage treatment plant is increased, and simultaneously, the great waste of resources is caused. Some enterprises also sell the waste lye to small paper mills cheaply and as a result are limited by the production conditions of the paper mills. When the paper mill is shut down or banned, the disposal of spent lye is limited. Therefore, in order to reduce the environmental protection pressure and the production cost, the purification and recovery treatment of the waste lye is a problem which must be solved by the continuous development of viscose fiber production enterprises.
Because the hemicellulose is a compound polysaccharide consisting of different monosaccharide groups, the molecular weight is small, the structure is complex, and simultaneously, the NaOH content of the waste alkali liquor is high, and the waste alkali liquor is difficult to recover and treat by adopting a conventional process. At present, the dialysis process and the membrane separation process are mainly adopted in China to purify and recover the waste alkali liquor, but the dialysis process has low alkali liquor recovery efficiency, large water consumption and large floor area and is gradually eliminated. In contrast, the membrane separation method has low cost and good effect and is being popularized and applied. However, the membrane separation method is actually a concentration process of hemicellulose in an aqueous alkali solution, and cannot completely and completely recover and recycle waste alkali liquor, and at least 30-50% of the waste alkali liquor needs to be treated by a traditional method.
Disclosure of Invention
Aiming at the defects of insufficient recovery and reutilization of waste alkali liquor in the viscose production process of the conventional chemical fiber plant, the invention aims to provide a method for recovering and reusing waste alkali liquor, which can completely recover and recycle waste alkali liquor in the viscose production process and can obtain a byproduct hemicellulose.
1. To achieve the purpose of the invention, the invention is realized by the following steps:
firstly, introducing viscose waste alkali liquor into a precipitation reactor, adding a hemicellulose precipitator, uniformly mixing, introducing supernatant into an intermediate tank after obvious layering of the solution occurs, and precipitating and separating out hemicellulose in the viscose waste alkali liquor.
And secondly, adding the precipitated hemicellulose into a solid-liquid separator, and performing solid-liquid separation to obtain solid hemicellulose and an aqueous solution containing a precipitator and sodium hydroxide.
Thirdly, drying the solid hemicellulose and simultaneously recovering the residual solvent and alkali liquor;
and fourthly, feeding the aqueous solution containing the precipitator and the sodium hydroxide into a rectifying tower to realize the separation of the alkali liquor and the precipitator in the rectifying tower. Discharging the precipitant from the top of the tower, returning to the first step for recycling, and recovering alkali liquor at the bottom of the tower;
and fifthly, returning the alkali liquor obtained in the third step and the fourth step to the viscose production flow for recycling.
And returning the alkali liquor obtained at the tower bottom to the viscose production flow for recycling.
2. The hemicellulose precipitant is an aqueous solution prepared by compounding an alcohol substance and a flocculating agent according to a mass ratio of 10:1 to 10000: 1.
3. The alcohol substance is methanol, ethanol, n-propanol, isopropanol or butanol or a mixed solvent;
4. the flocculating agent is polyacrylamide, aluminum sulfate, ammonium alum, ferric chloride, polyaluminium chloride or polyferric sulfate.
5. The volume ratio of the hemicellulose precipitant to the waste alkali liquor is 1: 1-10: 1, preferably 2: 1-4: 1. The reaction time for the hemicellulose precipitation is 1-100 minutes, and the precipitation temperature is from room temperature to the boiling temperature.
6. The precipitation reactor may be any vessel suitable for such reactions, the reaction being carried out at atmospheric pressure.
7. The hemicellulose solid-liquid separator may be any suitable device, such as a filter press, a vacuum drum filter, a centrifuge, a settling tank, a hydrocyclone, etc.
8. The separation of the hemicellulose precipitant from the lye can be carried out using any type of rectification apparatus, such as various plate columns and various packed columns.
The invention has the advantages that: after treatment, the content of hemicellulose in the waste liquid is reduced to below 15% of the initial content of the hemicellulose, so that the waste alkali liquor can be completely recovered and recycled, and a byproduct hemicellulose can be obtained. Not only is beneficial to energy conservation and emission reduction and environmental pollution reduction, but also can save a large amount of caustic soda, and is very beneficial to environmental protection.
Detailed Description
For a better illustration of the invention, the following examples are given:
example 1
1. And (2) introducing viscose waste alkali liquor (containing hemicellulose accounting for about 4 percent by mass and sodium hydroxide accounting for 20 percent by mass) into the precipitation reactor, adding a hemicellulose precipitator, uniformly mixing, standing for a period of time, introducing the supernatant into an intermediate tank after obvious layering of the solution occurs, and removing the supernatant to obtain hemicellulose slurry.
2. And (3) putting the hemicellulose slurry into a solid-liquid separator, separating the hemicellulose, washing and drying the solid hemicellulose, weighing and calculating the hemicellulose removal rate. The filtrate and washing liquid are water solution containing precipitant and sodium hydroxide, and are introduced into the intermediate tank to be combined with the supernatant.
3. Introducing the aqueous solution containing the precipitant and the sodium hydroxide into a rectifying tower, and separating the alkali liquor from the precipitant in the rectifying tower. And discharging the precipitator from the top of the tower, returning the precipitator to the first step for recycling, and returning the alkali liquor obtained at the bottom of the tower to the viscose production flow for recycling.
The hemicellulose precipitant is an aqueous solution prepared by compounding ethanol and polyacrylamide in a weight ratio of 100: 1.
Example 2
The procedure is as in example 1.
The hemicellulose precipitant is an aqueous solution prepared by compounding methanol and polymeric ferric sulfate according to the weight ratio of 1000: 1.
Example 3
The procedure is as in example 1.
The hemicellulose precipitant is a water solution prepared by compounding a mixed high-efficiency solvent and polymeric ferric sulfate according to the weight ratio of 1000: 1.
Claims (5)
1. The method for recycling the waste alkali liquor in the viscose fiber production process is characterized by comprising the following steps:
(1) introducing viscose waste alkali liquor into a precipitation reactor, adding a hemicellulose precipitator, uniformly mixing, introducing supernatant into an intermediate tank after obvious layering of the solution occurs, and precipitating and separating out hemicellulose in the viscose waste alkali liquor;
(2) putting the precipitated hemicellulose into a solid-liquid separation reaction kettle for solid-liquid separation to obtain solid hemicellulose and an aqueous solution containing a precipitator and sodium hydroxide;
(3) drying the solid hemicellulose, and simultaneously recovering the residual solvent and alkali liquor;
(4) introducing an aqueous solution containing a precipitator and sodium hydroxide into a rectifying tower, and separating alkali liquor from the precipitator in the rectifying tower; discharging the precipitant from the top of the tower, returning to the first step for recycling, and recovering alkali liquor at the bottom of the tower;
(5) and (4) returning the alkali liquor obtained in the steps (3) and (4) to the viscose production flow for recycling.
2. The hemicellulose precipitant is an aqueous solution prepared by compounding an alcohol substance and a flocculating agent in a weight ratio of 10:1 to 10000: 1.
3. The alcohol substance in claim 1 is methanol, ethanol, n-propanol, isopropanol or butanol or a mixed solvent.
4. The flocculant of claim 1 is polyacrylamide, aluminum sulfate, ammonium alum, ferric chloride, polyaluminum chloride or polyferric sulfate.
5. The method for recycling spent lye of claim 1 wherein the volume ratio of the hemicellulose precipitant to the spent lye is in the range of 1:1 to 10:1, preferably 1.5:1 to 4: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110377458.9A CN113023996A (en) | 2021-04-08 | 2021-04-08 | Recycling method of squeezed waste alkali liquor generated in viscose production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110377458.9A CN113023996A (en) | 2021-04-08 | 2021-04-08 | Recycling method of squeezed waste alkali liquor generated in viscose production |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113023996A true CN113023996A (en) | 2021-06-25 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110377458.9A Pending CN113023996A (en) | 2021-04-08 | 2021-04-08 | Recycling method of squeezed waste alkali liquor generated in viscose production |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113023996A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3405208A1 (en) * | 1983-02-24 | 1984-08-30 | Chemiefaser Lenzing AG, Lenzing, Oberösterreich | Process for the preparation of a water-binding agent based on hemicellulose, and the use of the agent |
| US5545418A (en) * | 1993-12-27 | 1996-08-13 | Kabushiki Kaisha Hayashibara Seibutsu Kagaku Kenkyujo | Alkali-treated bagasse, and its preparation and uses |
| CN102951712A (en) * | 2011-08-31 | 2013-03-06 | 天津滨海鼎昇环保科技工程有限公司 | Process for treating chemical wastewater by phenolphthalein coagulation |
| CN108047353A (en) * | 2017-12-20 | 2018-05-18 | 南京林业大学 | A kind of method of hemicellulose in separation in situ and recycling strong alkali solution |
| CN109735968A (en) * | 2018-12-18 | 2019-05-10 | 郑州家善环保科技有限公司 | A kind of spent lye recoverying and utilizing method |
| WO2020251463A1 (en) * | 2019-06-13 | 2020-12-17 | Treetotextile Ab | Fibers produced from recycled cellulosic waste material |
-
2021
- 2021-04-08 CN CN202110377458.9A patent/CN113023996A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3405208A1 (en) * | 1983-02-24 | 1984-08-30 | Chemiefaser Lenzing AG, Lenzing, Oberösterreich | Process for the preparation of a water-binding agent based on hemicellulose, and the use of the agent |
| US5545418A (en) * | 1993-12-27 | 1996-08-13 | Kabushiki Kaisha Hayashibara Seibutsu Kagaku Kenkyujo | Alkali-treated bagasse, and its preparation and uses |
| CN102951712A (en) * | 2011-08-31 | 2013-03-06 | 天津滨海鼎昇环保科技工程有限公司 | Process for treating chemical wastewater by phenolphthalein coagulation |
| CN108047353A (en) * | 2017-12-20 | 2018-05-18 | 南京林业大学 | A kind of method of hemicellulose in separation in situ and recycling strong alkali solution |
| CN109735968A (en) * | 2018-12-18 | 2019-05-10 | 郑州家善环保科技有限公司 | A kind of spent lye recoverying and utilizing method |
| WO2020251463A1 (en) * | 2019-06-13 | 2020-12-17 | Treetotextile Ab | Fibers produced from recycled cellulosic waste material |
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Application publication date: 20210625 |