CN105000742A - Waste alkali solution recycling method - Google Patents
Waste alkali solution recycling method Download PDFInfo
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- CN105000742A CN105000742A CN201510451500.1A CN201510451500A CN105000742A CN 105000742 A CN105000742 A CN 105000742A CN 201510451500 A CN201510451500 A CN 201510451500A CN 105000742 A CN105000742 A CN 105000742A
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- hemicellulose
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- waste lye
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Abstract
The invention belongs to the field of resource recycling and relates to a waste alkali solution recycling method, in particular to a method for cyclic utilization of waste alkali solutions in the viscose production process of chemical fiber factories. According to the waste alkali solution recycling method, hemicellulose is separated from the waste alkali solutions through a reaction unit, a solid-liquid separation unit and a rectification unit. Therefore, the waste alkali solutions can be completely recycled and cyclically utilized, meanwhile, the by-product hemicellulose can be obtained, the hemicellulose can be used as a raw material for producing furfural or xylose, and the additional value of waste liquor treatment is increased. Energy conservation and emission reduction are facilitated, environmental pollution is reduced, a large amount of caustic soda can be saved, and environmental protection is well facilitated.
Description
Technical field
The invention belongs to resource reutilization, be specifically related to the method for waste lye recycle in chemical fibre factory's production process of viscose fiber.
Background technology
Viscose fiber is one of main chemical fibre kind, and its output accounts for 1/3rd of global chemical fibre ultimate production.According to estimates, the viscose fiber production capacity of China is about 3,000,000 tons, and viscose fiber annual production accounts for 60% of Gross World Product.Along with the development of global economy and the growth of population, the consumption of viscose fiber still can continue to increase.Production process of viscose fiber comprises viscose glue preparation, spinning, aftertreatment and 4 stages of post-treatment, wherein need to consume a large amount of caustic soda in viscose glue preparation process, and producing a large amount of waste lyes, its main component is water, NaOH and hemicellulose, and wherein the content of NaOH is up to 17-20%.In production process of viscose fiber, alkali lye is recycle, but just can not be applied to production again when the hemicellulose concentration in alkali lye is elevated to a certain degree, otherwise the preparation process of viscose glue will be affected, and the quality of adhesive properties, molding condition and the finished product.In order to control the content of hemicellulose in alkali lye, original way is the content taking the mode of waste lye partial discharge to adjust hemicellulose in alkali lye, such needs consume a large amount of acid and neutralize, and have both increased the running cost of sewage work, cause the significant wastage of resource simultaneously.Also have Some Enterprises to sell little paper mill at an easy rate waste lye, result is limited by the production status in paper mill.When paper mill is closed down or banned, waste lye is disposed and is just restricted.Therefore, in order to alleviate environmental protection pressure, reduce production cost, carrying out the process of waste lye Recovery Purifying is the problem that the sustainable development of viscose fiber manufacturing enterprise must solve.
Due to the complex polysaccharide that hemicellulose is made up of different monosaccharide groups, molecular weight, complex structure, the NaOH content of waste lye is higher simultaneously, adopts common process to be difficult to recycling.Current China mainly adopts dialysis technique and membrane separation process to carry out Recovery Purifying waste lye, but dialysis technique reclaims alkali lye inefficiency, and water consumption is large, and floor space is large, progressively eliminates.Comparatively speaking, membrane separating method cost is low, effective, is widely applied.But membrane separating method is actually the concentration process of hemicellulose in alkali aqueous solution, it can not make waste lye reclaim for a full due and obtain recycle, has at least 30-50% waste lye also to use conventional process.
Summary of the invention
Reclaim for waste lye in current chemical fibre factory production process of viscose fiber, recycling is not enough, the object of the invention is to provide one
Plant the waste lye that waste lye in production process of viscose fiber can reclaim completely, recycle also can obtain byproduct hemicellulose and return sharp receipts method.
For realizing the object of the invention, the present invention realizes in the following way:
The first step, passes into viscose fiber waste lye in precipitation reactor, adds hemicellulose precipitation agent, mixes, and occurs, after layering, supernatant liquid being passed into medial launder until solution, the hemicellulose Precipitation in viscose fiber waste lye.
Second step, adds in solid-liquid separator by the hemicellulose of Precipitation, carries out solid-liquid separation, obtains solid hemicellulose and the aqueous solution containing precipitation agent and sodium hydroxide, passes in medial launder and merge with supernatant liquor.
3rd step, sends into the aqueous solution containing precipitation agent and sodium hydroxide in rectifying tower, realizes being separated of alkali lye and precipitation agent in rectifying tower.Precipitation agent is discharged by tower top, turns back to step one and carries out recycle, and the alkali lye obtained at the bottom of tower turns back to viscose glue Production Flow Chart and carries out recycle.
Above-mentioned hemicellulose precipitation agent is that alcohols material and flocculation agent are with 10:1 to 10000:1(weight part ratio) the composite aqueous solution.
Described alcohols material is methyl alcohol, ethanol, n-propyl alcohol, Virahol etc.
Described flocculation agent is polyacrylamide, Tai-Ace S 150, tschermigite, iron(ic) chloride, polymerize aluminum chloride, bodied ferric sulfate etc.
The volume ratio of hemicellulose precipitation agent and waste lye between 1:1-10:1, between preferred 2:1-4:1.The hemicellulose precipitin reaction time is 1-100 minute, and precipitation temperature is from room temperature to boiling temperature.
Precipitation reactor can be any container being suitable for this type of reaction, and reaction is carried out at ambient pressure.
Hemicellulose solid-liquid separator can adopt any suitable device, as pressure filter, vacuum-type drum filter, whizzer, subsider, wet cyclone etc.
Hemicellulose precipitation agent can adopt any type of rectifier unit with being separated of alkali lye, as various tray column and various packing tower.
The invention has the advantages that: through process, in waste liquid, hemicellulose level has dropped to less than 15% of its initial content, waste lye can be made to reclaim completely and recycle, byproduct hemicellulose can be obtained simultaneously, this hemicellulose can be used for the raw material producing furfural or wood sugar, adds liquid waste disposal added value.Not only be conducive to energy-saving and emission-reduction, reduce environmental pollution, and can a large amount of caustic soda be saved, be very beneficial for environment protection.
Accompanying drawing explanation
Fig. 1 is present invention process schema.
Embodiment
for better illustrating the present invention, as follows for embodiment:
embodiment 1
1, in precipitation reactor, pass into viscose fiber waste lye (containing the hemicellulose of mass percent about 4% and the sodium hydroxide of 20%), add hemicellulose precipitation agent, mix, leave standstill for some time, occur after obvious layering until solution, passed into by supernatant liquid in medial launder, removing supernatant liquid, obtains hemicellulose slurries.
2, hemicellulose slurries are inserted in solid-liquid separator, carry out hemicellulose separation, by the washing of solid hemicellulose, drying, weigh and calculate hemicellulose decreasing ratio, the results are shown in Table 1.Filtrate and washing lotion are the aqueous solution containing precipitation agent and sodium hydroxide, pass in medial launder and merge with supernatant liquor.
3, the aqueous solution containing precipitation agent and sodium hydroxide is passed in rectifying tower, in rectifying tower, realize being separated of alkali lye and precipitation agent.Precipitation agent is discharged by tower top, turns back to step one and carries out recycle, and the alkali lye obtained at the bottom of tower turns back to viscose glue Production Flow Chart and carries out recycle.
Above-mentioned hemicellulose precipitation agent be ethanol and polyacrylamide with 100:1 weight, the composite aqueous solution.
Table 1 alcohol settling removes hemicellulose result
| Waste lye: precipitation agent | Hemicellulose decreasing ratio/% | The precipitation agent rate of recovery/% | Recycle of alkali liquor rate/% |
| 1:1 | 50.0 | 99.8 | 100 |
| 1:1.5 | 66.7 | 99.6 | 100 |
| 1:2 | 75.3 | 99.5 | 100 |
| 1:3 | 85.5 | 99.5 | 100 |
| 1:4 | 85.0 | 99.5 | 100 |
| 1:5 | 55.6 | 99.5 | 100 |
| 1:10 | 48.5 | 99.8 | 100 |
embodiment 2
Above-mentioned hemicellulose precipitation agent be methyl alcohol and bodied ferric sulfate with 1000:1 weight, the composite aqueous solution.
Step is with embodiment 1.The results are shown in Table 2.
Table 2 methanol extraction removes hemicellulose result
| Waste lye: precipitation agent | Hemicellulose decreasing ratio/% | The precipitation agent rate of recovery/% | Recycle of alkali liquor rate/% |
| 1:1 | 35 | 99.8 | 100 |
| 1:1.5 | 45 | 99.6 | 100 |
| 1:2 | 60 | 99.5 | 100 |
| 1:2.5 | 75 | 99.5 | 100 |
| 1:3 | 85 | 99.5 | 100 |
| 1:4 | 85 | 99.5 | 100 |
| 1:5 | 75 | 99.6 | 100 |
Claims (3)
1. waste lye recoverying and utilizing method in production process of viscose fiber, is characterized in that, realizes by the following method:
(1) in precipitation reactor, pass into viscose fiber waste lye, add hemicellulose precipitation agent, mix, occur, after layering, supernatant liquid being passed into medial launder until solution, the hemicellulose Precipitation in viscose fiber waste lye;
(2) hemicellulose of Precipitation is inserted in solid-liquid separation reactor carry out solid-liquid separation, obtain solid hemicellulose and the aqueous solution containing precipitation agent and sodium hydroxide, pass in medial launder and merge with supernatant liquor;
(3) aqueous solution containing precipitation agent and sodium hydroxide is passed in rectifying tower, in rectifying tower, realize being separated of alkali lye and precipitation agent; Precipitation agent is discharged by tower top, turns back to step one and carries out recycle, and the alkali lye obtained at the bottom of tower turns back to viscose glue Production Flow Chart and carries out recycle;
Described hemicellulose precipitation agent is alcohols material and flocculation agent with the composite aqueous solution of 10:1 to 10000:1 weight;
Described alcohols material is methyl alcohol, ethanol, n-propyl alcohol or Virahol;
Described flocculation agent is polyacrylamide, Tai-Ace S 150, tschermigite, iron(ic) chloride, polymerize aluminum chloride or bodied ferric sulfate.
2. waste lye recoverying and utilizing method as claimed in claim 1, it is characterized in that, the volume ratio of hemicellulose precipitation agent and waste lye selects 1:1-10:1.
3. waste lye recoverying and utilizing method as claimed in claim 1, is characterized in that, the preferred 2:1-4:1 of volume ratio of hemicellulose precipitation agent and waste lye.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510451500.1A CN105000742A (en) | 2015-07-29 | 2015-07-29 | Waste alkali solution recycling method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510451500.1A CN105000742A (en) | 2015-07-29 | 2015-07-29 | Waste alkali solution recycling method |
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| CN105000742A true CN105000742A (en) | 2015-10-28 |
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| CN201510451500.1A Pending CN105000742A (en) | 2015-07-29 | 2015-07-29 | Waste alkali solution recycling method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108484798A (en) * | 2018-03-12 | 2018-09-04 | 南京林业大学 | A kind of methanol mediates the hydrophobic method efficiently separated with reuse alkaline solution and its dissolve hemicellulose |
| 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 |
| WO2019095698A1 (en) * | 2017-11-20 | 2019-05-23 | 中国科学院广州能源研究所 | Device for water saving and emission reduction technology of alkali-pretreated lignocellulose enzymolysis and saccharification |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1156126A (en) * | 1996-01-31 | 1997-08-06 | 迁安县华丰造纸厂 | Treatment method of papermaking black liquor |
| CN102585039A (en) * | 2012-02-28 | 2012-07-18 | 昆明理工大学 | Extraction separation method of hemicellulose |
| CN103333274A (en) * | 2013-07-11 | 2013-10-02 | 宜宾丝丽雅集团有限公司 | Method for extracting and recovering hemicellulose from squeezed waste alkali |
-
2015
- 2015-07-29 CN CN201510451500.1A patent/CN105000742A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1156126A (en) * | 1996-01-31 | 1997-08-06 | 迁安县华丰造纸厂 | Treatment method of papermaking black liquor |
| CN102585039A (en) * | 2012-02-28 | 2012-07-18 | 昆明理工大学 | Extraction separation method of hemicellulose |
| CN103333274A (en) * | 2013-07-11 | 2013-10-02 | 宜宾丝丽雅集团有限公司 | Method for extracting and recovering hemicellulose from squeezed waste alkali |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019095698A1 (en) * | 2017-11-20 | 2019-05-23 | 中国科学院广州能源研究所 | Device for water saving and emission reduction technology of alkali-pretreated lignocellulose enzymolysis and saccharification |
| CN108484798A (en) * | 2018-03-12 | 2018-09-04 | 南京林业大学 | A kind of methanol mediates the hydrophobic method efficiently separated with reuse alkaline solution and its dissolve hemicellulose |
| 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 |
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Application publication date: 20151028 |