CN109183199A - A kind of NMMO solvent recovery method for concentration - Google Patents
A kind of NMMO solvent recovery method for concentration Download PDFInfo
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- CN109183199A CN109183199A CN201811396975.5A CN201811396975A CN109183199A CN 109183199 A CN109183199 A CN 109183199A CN 201811396975 A CN201811396975 A CN 201811396975A CN 109183199 A CN109183199 A CN 109183199A
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- concentration
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F13/00—Recovery of starting material, waste material or solvents during the manufacture of artificial filaments or the like
- D01F13/02—Recovery of starting material, waste material or solvents during the manufacture of artificial filaments or the like of cellulose, cellulose derivatives or proteins
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of NMMO solvent recovery method for concentration, which comprises the following steps: S1: recycling NMMO rinsing solution is to adjusting tank；S2: measurement recycling index of refraction；S3: being added distilled water until index of refraction is 1.3~1.4；S4: enter the first concentration tank, 100~120 DEG C of temperature, vacuum degree be -30~-40KPa, concentration time 3~5 hours；S5: enter the second concentration tank, 105~130 DEG C of temperature, vacuum degree be -50~-65KPa, concentration time 3~5 hours；S6: enter third concentration tank, 140~150 DEG C of temperature, vacuum degree be -70~-80KPa, concentration time 3~5 hours；S7: enter evaporator, 160 DEG C of temperature, vacuum degree is -90~-100KPa, until index of refraction is 1.45~1.52.By above-mentioned recycling method for concentration, the generation of natural fiber long filament can ensure that while guaranteeing to recycle NMMO solution, reduce cost, reduce pollution.
Description
Technical field
The present invention relates to textile fabric field more particularly to a kind of NMMO solvent recovery method for concentration.
Background technique
Cellulose fibre refers to all fibers obtained by cellulosic polymer, is divided into native cellulose fibre and regeneration is fine
Cellulose fiber.Due to arable land reduction and petroleum resources it is increasingly depleted, natural fiber, synthetic fibers yield will will receive more
Carry out more restrictions；People pay attention to textile process of consumption in environmental-protecting performance while, to the value of regenerated celulose fibre
It is re-recognized and has been excavated.Nowadays the application of regenerated celulose fibre has obtained a unprecedented opportunity to develop.Tradition
Regenerated celulose fibre use pulp for base stock, soluble cellulose yellow acid is made through processes such as alkalization, aging, sulfonation
Ester is re-dissolved in sig water, is made through wet spinning.In the technique of production cellulose fibre, it is common to use N-methylmorpholine-
The aqueous solution of N- oxide (i.e. NMMO) is as swelling solvent.In this traditional preparation process, maximum defect is made
Think that fiber can only be the staple fiber that length is 30~36 centimetres, leading spinning is needed when being woven into cloth, workload is huge, and holds
Easy fracture of wire, while NMMO solution usage amount is huge every time, cost is high.
Summary of the invention
In order to solve the above-mentioned technical problem, the purpose of the present invention is to provide a kind of NMMO solvent recovery method for concentration.
To achieve the goals above, the technical scheme adopted by the invention is as follows: a kind of NMMO solvent recovery method for concentration, packet
Include following steps:
S1: recycling NMMO rinsing solution is to adjusting tank；
S2: measurement recycling index of refraction；
S3: being added distilled water until index of refraction is 1.3~1.4；
S4: enter the first concentration tank, 100~120 DEG C of temperature, vacuum degree is -30~-40KPa, and concentration time 3~5 is small
When；
S5: enter the second concentration tank, 105~130 DEG C of temperature, vacuum degree is -50~-65KPa, and concentration time 3~5 is small
When；
S6: enter third concentration tank, 140~150 DEG C of temperature, vacuum degree is -70~-80KPa, and concentration time 3~5 is small
When；
S7: enter evaporator, 160 DEG C of temperature, vacuum degree is -90~-100KPa, until index of refraction is 1.45~1.52.
By the above method, the NMMO rinsing solution being diluted by washing can be concentrated into can be again to natural
The NMMO solution of fiber swelling.
Preferably, after S3 meets technique requirement, 60% concentration hydrogen peroxide 0.05~1.2% (mass percent) is added.
By adding the addition of hydrogen peroxide, the oxidation impurities in NMMO solution can be restored.
Preferably, it after S7 meets technique requirement, is added azanol 0.3~0.5% (mass percent).
By the addition of azanol, complex compound can be formed with the metal ion in solution, reduce metal ion and impurity pair
The destruction of NMMO solution ensure that impurity reduces in fiber filament, can form long fibre.
Preferably, the index of refraction is measured by abbe's refractometer.
Compared with the prior art, the advantages of the present invention are as follows: by above-mentioned recycling method for concentration, it can guarantee circulation benefit
With NMMO solution, reduce cost, reduce pollution while, ensure that the generation of natural fiber long filament.
Specific embodiment
Present invention is further described in detail by the following examples.
Embodiment one
Technical solution used by the present embodiment are as follows:
A kind of NMMO solvent recovery method for concentration, which comprises the following steps:
Step 1: recycling NMMO rinsing solution is to adjusting tank；
Step 2: measurement recycling index of refraction；
Step 3: distilled water is added until measuring index of refraction by abbe's refractometer is 1.3；
Step 31: 60% concentration hydrogen peroxide 0.05% (mass percent) is added；
Step 4: enter the first concentration tank, 100 DEG C of temperature, vacuum degree be -40KPa, concentration time 5 hours；
Step 5: enter the second concentration tank, 105 DEG C of temperature, vacuum degree be -65KPa, concentration time 5 hours；
Step 6: enter third concentration tank, 140 DEG C of temperature, vacuum degree be -80KPa, concentration time 5 hours；
Step 7: entering evaporator, 160 DEG C of temperature, vacuum degree is -100KPa, until index of refraction is 1.49；
Step 71: being added azanol 0.5% (mass percent).
Embodiment two
Technical solution used by the present embodiment are as follows:
A kind of NMMO solvent recovery method for concentration, which comprises the following steps:
Step 1: recycling NMMO rinsing solution is to adjusting tank；
Step 2: measurement recycling index of refraction；
Step 3: distilled water is added until measuring index of refraction by abbe's refractometer is 1.4；
Step 31: 60% concentration hydrogen peroxide 1.2% (mass percent) is added；
Step 4: enter the first concentration tank, 120 DEG C of temperature, vacuum degree be -30KPa, concentration time 3 hours；
Step 5: enter the second concentration tank, 130 DEG C of temperature, vacuum degree be -50KPa, concentration time 3 hours；
Step 6: enter third concentration tank, 150 DEG C of temperature, vacuum degree be -70KPa, concentration time 3 hours；
Step 7: entering evaporator, 160 DEG C of temperature, vacuum degree is -90KPa, until index of refraction is 1.48；
Step 71: being added azanol 0.3% (mass percent).
Embodiment three
Technical solution used by the present embodiment are as follows:
A kind of NMMO solvent recovery method for concentration, which comprises the following steps:
Step 1: recycling NMMO rinsing solution is to adjusting tank；
Step 2: measurement recycling index of refraction；
Step 3: distilled water is added until measuring index of refraction by abbe's refractometer is 1.33；
Step 31: 60% concentration hydrogen peroxide 0.625% (mass percent) is added；
Step 4: enter the first concentration tank, 110 DEG C of temperature, vacuum degree be -35KPa, concentration time 4 hours；
Step 5: enter the second concentration tank, 117 DEG C of temperature, vacuum degree be -57KPa, concentration time 4 hours；
Step 6: enter third concentration tank, 145 DEG C of temperature, vacuum degree be -75KPa, concentration time 4 hours；
Step 7: entering evaporator, 160 DEG C of temperature, vacuum degree is -95KPa, until index of refraction is 1.50；
Step 71: being added azanol 0.4% (mass percent).
Example IV
Technical solution used by the present embodiment are as follows:
A kind of NMMO solvent recovery method for concentration, which comprises the following steps:
Step 1: recycling NMMO rinsing solution is to adjusting tank；
Step 2: measurement recycling index of refraction；
Step 3: distilled water is added until measuring index of refraction by abbe's refractometer is 1.36；
Step 31: 60% concentration hydrogen peroxide 0.3% (mass percent) is added；
Step 4: enter the first concentration tank, 105 DEG C of temperature, vacuum degree be -37KPa, concentration time 4.6 hours；
Step 5: enter the second concentration tank, 110 DEG C of temperature, vacuum degree be -60KPa, concentration time 4.5 hours；
Step 6: enter third concentration tank, 143 DEG C of temperature, vacuum degree be -77KPa, concentration time 4.5 hours；
Step 7: entering evaporator, 160 DEG C of temperature, vacuum degree is -97KPa, until index of refraction is 1.49；
Step 71: being added azanol 0.45% (mass percent).
Embodiment five
Technical solution used by the present embodiment are as follows:
A kind of NMMO solvent recovery method for concentration, which comprises the following steps:
Step 1: recycling NMMO rinsing solution is to adjusting tank；
Step 2: measurement recycling index of refraction；
Step 3: distilled water is added until measuring index of refraction by abbe's refractometer is 1.38；
Step 31: 60% concentration hydrogen peroxide 0.8% (mass percent) is added；
Step 4: enter the first concentration tank, 115 DEG C of temperature, vacuum degree be -33KPa, concentration time 3.4 hours；
Step 5: enter the second concentration tank, 122 DEG C of temperature, vacuum degree be -54KPa, concentration time 3.8 hours；
Step 6: enter third concentration tank, 147 DEG C of temperature, vacuum degree be -72KPa, concentration time 3.6 hours；
Step 7: entering evaporator, 160 DEG C of temperature, vacuum degree is -93KPa, until index of refraction is 1.48；
Step 71: being added azanol 0.35% (mass percent).
Embodiment six
Technical solution used by the present embodiment are as follows:
A kind of NMMO solvent recovery method for concentration, which comprises the following steps:
Step 1: recycling NMMO rinsing solution is to adjusting tank；
Step 2: measurement recycling index of refraction；
Step 3: distilled water is added until measuring index of refraction by abbe's refractometer is 1.3；
Step 31: 60% concentration hydrogen peroxide 0.05% (mass percent) is added；
Step 4: enter the first concentration tank, 100 DEG C of temperature, vacuum degree be -30KPa, concentration time 3 hours；
Step 5: enter the second concentration tank, 105 DEG C of temperature, vacuum degree be -50KPa, concentration time 3 hours；
Step 6: enter third concentration tank, 140 DEG C of temperature, vacuum degree be -70KPa, concentration time 3 hours；
Step 7: entering evaporator, 160 DEG C of temperature, vacuum degree is -90KPa, until index of refraction is 1.45；
Step 71: being added azanol 0.5% (mass percent).
Embodiment seven
Technical solution used by the present embodiment are as follows:
A kind of NMMO solvent recovery method for concentration, which comprises the following steps:
Step 1: recycling NMMO rinsing solution is to adjusting tank；
Step 2: measurement recycling index of refraction；
Step 3: distilled water is added until measuring index of refraction by abbe's refractometer is 1.4；
Step 31: 60% concentration hydrogen peroxide 1.2% (mass percent) is added；
Step 4: enter the first concentration tank, 120 DEG C of temperature, vacuum degree be -40KPa, concentration time 5 hours；
Step 5: enter the second concentration tank, 130 DEG C of temperature, vacuum degree be -65KPa, concentration time 5 hours；
Step 6: enter third concentration tank, 150 DEG C of temperature, vacuum degree be -80KPa, concentration time 5 hours；
Step 7: entering evaporator, 160 DEG C of temperature, vacuum degree is -90KPa, until index of refraction is 1.52；
Step 71: being added azanol 0.3% (mass percent).
Although the preferred embodiment of the present invention has been described in detail above, it is to be clearly understood that for this field
Technical staff for, the invention may be variously modified and varied.Done within the spirit and principles of the present invention
What modification, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (4)
1. a kind of NMMO solvent recovery method for concentration, which comprises the following steps:
S1: recycling NMMO rinsing solution is to adjusting tank；
S2: measurement recycling index of refraction；
S3: being added distilled water until index of refraction is 1.3~1.4；
S4: enter the first concentration tank, 100~120 DEG C of temperature, vacuum degree be -30~-40KPa, concentration time 3~5 hours；
S5: enter the second concentration tank, 105~130 DEG C of temperature, vacuum degree be -50~-65KPa, concentration time 3~5 hours；
S6: enter third concentration tank, 140~150 DEG C of temperature, vacuum degree be -70~-80KPa, concentration time 3~5 hours；
S7: enter evaporator, 160 DEG C of temperature, vacuum degree is -90~-100KPa, until index of refraction is 1.45~1.52.
2. NMMO solvent recovery method for concentration according to claim 1, which is characterized in that after S3 meets technique requirement,
60% concentration hydrogen peroxide 0.05~1.2% (mass percent) is added.
3. NMMO solvent recovery method for concentration according to claim 1, it is characterised in that: after S7 meets technique requirement,
It is added azanol 0.3~0.5% (mass percent).
4. NMMO solvent recovery method for concentration according to claim 1, which is characterized in that the index of refraction is rolled over by Abbe
The measurement of light instrument.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110670163A (en) * | 2019-10-12 | 2020-01-10 | 淮安天然丝纺织科技有限公司 | NMMO solution suitable for cellulose filament fiber and preparation method of cellulose filament fiber using NMMO solution |
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| EP0679739A1 (en) * | 1994-04-27 | 1995-11-02 | Korea Institute Of Science And Technology | Method for the purification of reclaimed aqueous N-methylmorpholine N-oxide solution |
| CN101280476A (en) * | 2008-05-23 | 2008-10-08 | 宜宾丝丽雅集团有限公司 | Recovery method for NMMO solvent in fibre production by solvent method |
| CN101942713A (en) * | 2009-07-07 | 2011-01-12 | 中国科学院化学研究所 | Recovery method of N-methylmorpholine oxide solvent in process of generating regenerated protein fibre by solvent method |
| CN101942712A (en) * | 2009-07-07 | 2011-01-12 | 中国科学院化学研究所 | Recovery method of N-methylmorpholine oxide solvent in process of producing regenerated cellulose fibre by solvent method |
| CN102234852A (en) * | 2010-04-21 | 2011-11-09 | 聚隆纤维股份有限公司 | Solvent recovery method of Lyocell fibers |
| CN102758273A (en) * | 2011-04-28 | 2012-10-31 | 聚隆纤维股份有限公司 | Efficient energy-saving N-methylmorpholine-N-oxide solvent recovery method |
| CN104177536A (en) * | 2014-07-25 | 2014-12-03 | 南京大学 | Chelating resin adsorbing material and preparation method thereof |
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2018
- 2018-11-22 CN CN201811396975.5A patent/CN109183199A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0679739A1 (en) * | 1994-04-27 | 1995-11-02 | Korea Institute Of Science And Technology | Method for the purification of reclaimed aqueous N-methylmorpholine N-oxide solution |
| CN101280476A (en) * | 2008-05-23 | 2008-10-08 | 宜宾丝丽雅集团有限公司 | Recovery method for NMMO solvent in fibre production by solvent method |
| CN101942713A (en) * | 2009-07-07 | 2011-01-12 | 中国科学院化学研究所 | Recovery method of N-methylmorpholine oxide solvent in process of generating regenerated protein fibre by solvent method |
| CN101942712A (en) * | 2009-07-07 | 2011-01-12 | 中国科学院化学研究所 | Recovery method of N-methylmorpholine oxide solvent in process of producing regenerated cellulose fibre by solvent method |
| CN102234852A (en) * | 2010-04-21 | 2011-11-09 | 聚隆纤维股份有限公司 | Solvent recovery method of Lyocell fibers |
| CN102758273A (en) * | 2011-04-28 | 2012-10-31 | 聚隆纤维股份有限公司 | Efficient energy-saving N-methylmorpholine-N-oxide solvent recovery method |
| CN104177536A (en) * | 2014-07-25 | 2014-12-03 | 南京大学 | Chelating resin adsorbing material and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110670163A (en) * | 2019-10-12 | 2020-01-10 | 淮安天然丝纺织科技有限公司 | NMMO solution suitable for cellulose filament fiber and preparation method of cellulose filament fiber using NMMO solution |
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| TA01 | Transfer of patent application right |
Effective date of registration: 20200611 Address after: Room 201-2, building 2, No. 290, Xingci first road, Hangzhou Bay New District, Ningbo City, Zhejiang Province Applicant after: Zhejiang lonsel Fiber Technology Co., Ltd Address before: 223400 Lianshui County of Huaian City, Jiangsu Province Industrial District West Road on the north side of glory Applicant before: NUFIBER (HUAI'AN) TEXTILE TECHNOLOGY Co.,Ltd. |
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Application publication date: 20190111 |