CN111074384B - Method for recovering N-methylmorpholine oxide solvent in Lyocell fiber regenerated acid and preparation method of solvent - Google Patents
Method for recovering N-methylmorpholine oxide solvent in Lyocell fiber regenerated acid and preparation method of solvent Download PDFInfo
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- CN111074384B CN111074384B CN201911237058.7A CN201911237058A CN111074384B CN 111074384 B CN111074384 B CN 111074384B CN 201911237058 A CN201911237058 A CN 201911237058A CN 111074384 B CN111074384 B CN 111074384B
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- 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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Abstract
Discloses a method for recovering an N-methylmorpholine oxide solvent in Lyocell fiber regenerated acid and a method for preparing the N-methylmorpholine oxide solvent, belonging to the technical field of industrial emission reduction. The method for recovering the N-methylmorpholine oxide solvent in the Lyocell fiber regenerated acid comprises the following steps: collecting the Lyocell fiber regenerated acid as a waste hydrochloric acid solution; the waste acid solution is subjected to activated carbon adsorption treatment to obtain a first intermediate product; and (3) carrying out nanofiltration treatment on the first intermediate product to obtain the recovered N-methylmorpholine oxide solvent. The preparation method of the N-methylmorpholine oxide solvent comprises the following steps: and blending the N-methylmorpholine oxide solvent recovered by the method for recovering the N-methylmorpholine oxide solvent from the Lyocell fiber regenerated acid with hydrochloric acid to obtain the N-methylmorpholine oxide solvent with the concentration of hydrochloric acid according with cation regeneration. The method can realize the purification and cyclic utilization of the waste hydrochloric acid, and simultaneously recovers the high-cost NMMO in the waste hydrochloric acid so as to reduce the loss of the NMMO solvent in the solvent recovery process of Lyocell fiber production.
Description
Technical Field
The invention relates to the technical field of industrial emission reduction, in particular to a method for recovering an N-methylmorpholine oxide solvent in Lyocell fiber regenerated acid and a method for preparing the N-methylmorpholine oxide solvent.
Background
The aqueous solution of N-methylmorpholine oxide (NMMO) is a high-quality solvent in the green fiber manufacturing process, the fiber prepared by dissolving cellulose by using NMMO as a solvent is called Lyocell fiber, a large amount of NMMO solvent is used in the existing production, the production process is green in circulation and takes the production cost into consideration, the NMMO solvent is diluted from higher concentration to lower concentration in the fiber production process, and a large amount of NMMO exists in a low-concentration solvent, so that the solvent recovery process is indispensable in the Lyocell fiber production. In the solvent recovery engineering, how to maximize the recovery rate of NMMO and reduce the emission loss of NMMO is one of the key problems in the development of solvent-process fibers at present.
Disclosure of Invention
In view of the above, the invention provides a method for recovering an N-methylmorpholine oxide solvent from Lyocell fiber regenerated acid and a method for preparing the N-methylmorpholine oxide solvent, which can realize the purification and cyclic utilization of waste hydrochloric acid, and simultaneously recover high-cost NMMO from the waste hydrochloric acid to reduce the loss of the NMMO solvent in the solvent recovery process in Lyocell fiber production, thereby being more practical.
In order to achieve the first purpose, the technical scheme of the method for recovering the N-methylmorpholine oxide solvent in the Lyocell fiber regenerated acid provided by the invention is as follows:
the invention provides a method for recovering an N-methylmorpholine oxide solvent in Lyocell fiber regenerated acid, which comprises the following steps:
collecting the Lyocell fiber regenerated acid as a waste hydrochloric acid solution;
adsorbing the waste acid solution by using activated carbon to obtain a first intermediate product;
and carrying out nanofiltration treatment on the first intermediate product to obtain the recovered N-methylmorpholine oxide solvent.
The method for recovering the N-methylmorpholine oxide solvent in the Lyocell fiber regenerated acid can be further realized by adopting the following technical measures.
As a preference, the first and second liquid crystal compositions are,
in the nanofiltration treatment process, the intercepted concentrated solution is led to a sewage treatment system for sewage treatment, and the intermediate permeate liquid after nanofiltration is recycled for nanofiltration treatment until the final permeate liquid containing the N-methylmorpholine oxide solvent hydrochloric acid is discharged, so as to obtain the recovered N-methylmorpholine oxide solvent.
Preferably, in the process of obtaining the first intermediate product by adsorbing the waste acid solution by activated carbon,
the flow rate of the waste acid solution ranges from 3BV/h to 7 BV/h;
The retention time of the waste acid solution in the activated carbon adsorption treatment system is within a value range of 3-5 min.
Preferably, in the process of obtaining the recovered N-methylmorpholine oxide solvent by subjecting the first intermediate product to nanofiltration,
the flow rate of the first intermediate product ranges from 4BV/h to 8 BV/h;
the value range of the process pressure in the nanofiltration treatment process is 3 MPa-7 MPa;
the flow rate of the intermediate permeate and the final permeate ranges from 2BV/h to 7 BV/h.
As a preference, the first and second liquid crystal compositions are,
and in the nanofiltration treatment process, the first intermediate product enters a nanofiltration treatment system in a pump conveying mode.
As a preference, the first and second liquid crystal compositions are,
the active carbon is powder active carbon with holes,
the activated carbon is uniformly filled in the activated carbon treatment system.
In order to achieve the second object, the technical scheme of the preparation method of the N-methylmorpholine oxide solvent provided by the invention is as follows:
the preparation method of the N-methylmorpholine oxide solvent provided by the invention comprises the following steps:
the N-methylmorpholine oxide solvent recovered by the method provided by the invention is mixed with hydrochloric acid to obtain the N-methylmorpholine oxide solvent with the concentration of hydrochloric acid according with cation regeneration.
The invention has the beneficial effects that: compared with the prior art, the method has the advantages that the part of waste hydrochloric acid solution in the production process is used as engineering sewage and directly enters a neutralization system to be discharged into a sewage treatment system, and a certain amount of NMMO solvent contained in the waste hydrochloric acid solution is directly discharged along with the sewage, so that the direct loss of the NMMO is caused. The cation exchange resin in the solvent recovery process in Lyocell fiber production can adsorb a certain amount of solvent NMMO for dissolving cellulose, and after the cation exchange resin is saturated, the cation exchange resin needs to be washed by hydrochloric acid, so that the cation exchange resin returns to an ion active state again, and in the waste hydrochloric acid solution for regenerating the cation exchange resin, not only can the impurities adsorbed on the cation exchange resin be eluted, but also the solvent NMMO adsorbed on the cation exchange resin is washed away, so that the waste hydrochloric acid solution for regenerating the ion resin contains a certain amount of NMMO solvent. The hydrochloric acid permeate liquid treated by the activated carbon and nanofiltration technology contains NMMO solvent, and the hydrochloric acid can be reused for concentration blending to meet the concentration of the hydrochloric acid for cation regeneration, and then is continuously recycled to carry out acid regeneration on the cation exchange resin. Through this technical scheme, realize the cyclic utilization of NMMO solvent, make the NMMO solvent that retrieves in the acid always exist in the recovery system, effectively reduce NMMO solvent loss in green fiber production, improved NMMO solvent recovery efficiency.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to refer to like parts throughout the drawings. In the drawings:
FIG. 1 is a flow chart showing the change of substances in the method for recovering the solvent of N-methylmorpholine oxide from the regenerated acid of Lyocell fiber and the method for preparing the solvent of N-methylmorpholine oxide.
Detailed Description
The invention aims to solve the problems in the prior art and provides a method for recovering an N-methylmorpholine oxide solvent in Lyocell fiber regenerated acid, which can realize the purification and cyclic utilization of waste hydrochloric acid and simultaneously recover high-cost NMMO in the waste hydrochloric acid so as to reduce the loss of the NMMO solvent in the solvent recovery process in the production of Lyocell fibers, thereby being more practical.
To further illustrate the technical means and effects of the present invention for achieving the predetermined objects, the following detailed description of the solvent recovery method of N-methylmorpholine oxide from Lyocell fiber regenerated acid according to the present invention with reference to the accompanying drawings and preferred embodiments will be made as follows. In the following description, different "one embodiment" or "an embodiment" refers to not necessarily the same embodiment. Furthermore, the features, structures, or characteristics of one or more embodiments may be combined in any suitable manner.
The term "and/or" herein is merely an association describing an associated object, meaning that three relationships may exist, e.g., a and/or B, with the specific understanding that: both a and B may be included, a may be present alone, or B may be present alone, and any of the three cases can be provided.
According to the invention, the activated carbon adsorption process and the nanofiltration acid recovery device are connected in series to carry out the recovery operation of the NMMO solvent in the waste hydrochloric acid solution regenerated by the ionic resin, so that the recovery and utilization of the NMMO solvent contained in the waste hydrochloric acid solution can be realized, and the discharge loss is reduced. The method for recovering the NMMO solvent from the waste hydrochloric acid comprises the following steps:
1. the discharged waste hydrochloric acid after being treated by the cation exchange resin is intensively recycled into a storage tank for mixing and storage;
2. adsorbing organic substances with specific molecular weights by using the waste hydrochloric acid solution raw material obtained in the step 1 through an activated carbon adsorption process at a flow rate of 3-7 BV/h, and controlling the retention time of the solution in the system to be 3-5 min;
3. introducing the liquid discharged in the step 2 into a nanofiltration recovery process at a ratio of 4 BV/h-8 BV/h, introducing the waste hydrochloric acid solution into equipment at a pump frequency of 15 Hz-25 Hz, continuously filtering and circulating under the condition of increasing the pressure of 3-7 MPa, continuously discharging at a flow rate of 2 BV/h-7 BV/h, and completely removing other impurities except NMMO in the waste hydrochloric acid solution; separating NMMO solvent and hydrochloric acid from the permeate;
4. And (4) conveying the clear colorless transparent hydrochloric acid solution obtained in the step (3) to a hydrochloric acid blending storage tank, and adding a part of concentrated hydrochloric acid solution to re-blend and regenerate a new hydrochloric acid solution.
5. And (3) respectively carrying out acid concentration test, impurity component content test, NMMO solvent content test and chroma test on the discharged material samples in the steps 1, 2 and 3.
The activated carbon is in the form of fine powder with special type micropores, and is uniformly distributed in the absorption device through the filler.
The nanofiltration recovery material can selectively permeate organic substances with the molecular weight lower than 200, inorganic hydrochloric acid can completely permeate the organic substances, the material can not corrode and damage the material after long-term use of acidic liquid, and the nanofiltration system is provided with heat exchange equipment for preventing the material liquid from being overheated circularly for a long time, so that the material liquid can be timely exchanged heat in the process of large-scale circulation of the hydrochloric acid solution, the internal components are changed, and the NMMO and other components are decomposed.
The booster pump and the delivery pump for the hydrochloric acid solution are both made of acid-resistant materials, and can prevent acid corrosion after long-term use.
And stopping acid discharging when the circulating process of the equipment reaches a certain concentration, wherein non-target impurities are contained in the circulating residual liquid and are directly discharged to a sewage treatment working section.
The clean acid solution treated by the equipment contains a part of NMMO solvent, and is reused in a Lyocell fiber solvent recovery system, so that the loss of the solvent is reduced.
The invention is further illustrated by the following examples, which are intended to be illustrative only and are not intended to be in any way limiting.
Example one
NMMO recovery treatment is carried out on regenerated waste hydrochloric acid obtained after solvent recovery of styrene strong acid type gel cation exchange resin, and the steps are as follows:
1. regenerated waste hydrochloric acid (acid concentration is 10.5%, NMMO solvent concentration is 8%, weight is 250 kg) is discharged from a discharge port at the lower part of the cation exchange resin equipment and is put into a waste hydrochloric acid storage tank.
2. The waste hydrochloric acid raw material enters an activated carbon adsorption process at the flow rate of 3BV/h, the solution is circularly filtered in the activated carbon, the retention time is kept at 3min, and then the material is discharged through the activated carbon adsorption process.
3. Pumping the liquid treated by the activated carbon into a front feed inlet of a nanofiltration recovery treatment device at the flow rate of 4 BV/h;
4. the treated hydrochloric acid solution is conveyed to the nanofiltration recovery process at a flow rate of 7BV/h by adjusting the frequency of a booster pump in the system to 17 Hz.
5. The internal pressure of the device is increased to 3MPa, and the filtered acid liquor is discharged at the flow rate of 4BV/h through the equipment.
6. The filtered acid liquor is conveyed to an acid blending tank by a pump and is reused for the regeneration of the cation exchange resin after being blended into acid solution with certain concentration.
The test method is as follows:
1. acid concentration test: and (3) performing acid-base titration, namely taking a 2mL acid solution sample of a standard solution NaOH (1mol/L), adding a drop of methyl orange indicator, performing base titration until the color of methyl red changes, and calculating to obtain the concentration of hydrochloric acid.
2. NMMO concentration test: high Performance Liquid Chromatography (HPLC) test comprises adjusting pH of sample solution to about 7, making mobile phase be 10mmol/L methanol water solution, setting wavelength of ultraviolet detector 205nm, sampling amount to 20 μ L, and quantifying by external standard method.
3. And (3) testing the chromaticity: the color of the samples taken from each fraction was measured according to the method of GB 11903-1989.
In the embodiment, after the waste hydrochloric acid raw material is treated through the activated carbon and nanofiltration recovery process, liquid chromatography tests show that other impurities except NMMO in the solution are removed in the filtration recovery system, after 250kg of raw material waste acid is treated, 213kg of hydrochloric acid solution can be recovered, samples before and after acid-base titration show that 100% recovery of hydrochloric acid can be realized, the recovery rate of NMMO solvent reaches up to 88.4%, the emission of acid wastewater containing color of 85.2% is reduced, and the chromaticity of the waste acid solution is effectively reduced through treatment. By using the hydrochloric acid solution, the regenerated solution is prepared by using the hydrochloric acid again, and the cation exchange resin is washed, so that the purchase and use of the hydrochloric acid solution can be effectively reduced, the hydrochloric acid is effectively recycled, most of the NMMO solvent is recovered, and the loss rate of the high-cost solvent is effectively reduced.
Example two
The method comprises the following steps of carrying out NMMO recovery treatment on the regenerated acid obtained by recovering a solvent from a styrene strong acid type macroporous FC cation exchange resin:
1. regenerated waste hydrochloric acid (with the concentration of 7.7 percent and the NMMO solvent concentration of 12 percent and the weight of 250 kilograms) is discharged from a discharge hole at the lower part of the cation exchange resin equipment and is put into a waste hydrochloric acid storage tank.
2. The waste hydrochloric acid raw material enters an activated carbon adsorption process at the flow rate of 7BV/h, the solution is circularly filtered in the activated carbon, the retention time is kept at 5min, and then the waste hydrochloric acid raw material is discharged through the activated carbon adsorption process.
3. The liquid filtered by the activated carbon passes through the feed of the nanofiltration recovery process at the flow rate of 8 BV/h.
4. The frequency of the liquid is adjusted to 20Hz by a booster pump, and the liquid is conveyed to the nanofiltration recovery process at the flow rate of 6 BV/h.
5. The internal pressure of the device is increased to 4MPa, and the filtered acid liquor is discharged at the flow rate of 7BV/h through the equipment.
6. The filtered acid solution is conveyed to an acid blending tank by a pump and is blended into an acid solution with a certain concentration and then is reused for the regeneration of the cation exchange resin.
The test method is as follows:
1. acid concentration test: and (3) performing acid-base titration, namely taking a 2mL acid solution sample of a standard solution NaOH (1mol/L), adding a drop of methyl orange indicator, performing base titration until the color of methyl red changes, and calculating to obtain the concentration of hydrochloric acid.
2. NMMO concentration test: high Performance Liquid Chromatography (HPLC) test comprises adjusting pH of sample solution to about 7, making mobile phase be 10mmol/L methanol water solution, setting wavelength of ultraviolet detector 205nm, sampling amount to 20 μ L, and quantifying by external standard method.
3. And (3) testing the chromaticity: the color of the samples taken from each fraction was measured according to the method of GB 11903-1989.
In this embodiment, the adsorption performance of the cation exchange resin is good, more hydrogen ions are replaced by the hydrochloric acid solution, the concentration of consumed hydrochloric acid is high, the concentration of the waste hydrochloric acid solution is 7.7%, more NMMO adsorbed on the cation exchange resin is eluted by hydrochloric acid, so that the content of NMMO in the waste hydrochloric acid is increased by 12%, the chromaticity of the waste acid solution is also high, through the adsorption of active carbon, more retention time is needed to realize the adsorption of organic impurities with specific molecular weight, the hydrochloric acid solution is discharged and then passes through the nanofiltration recovery process, because the concentration of NMMO in the feed is high, the internal pressure of the system is correspondingly increased, the acid permeation flow rate is increased accordingly, more effective nanofiltration treatment is realized, the permeation liquid is tested, the NMMO content is improved, the NMMO recovery rate is up to 88.9%, and the hydrochloric acid is also realized to permeate 100%. In addition, the processing capacity of the waste acid raw material is 250kg, the collection weight of the treated discharged hydrochloric acid solution is 192kg, and the sewage discharge amount is effectively reduced by 76.8%.
EXAMPLE III
The method comprises the following steps of carrying out NMMO recovery treatment on the regenerated acid obtained by recovering a solvent from a styrene strong acid type homogeneous cation exchange resin:
1. regenerated waste hydrochloric acid (the concentration is 4.8 percent, the NMMO solvent concentration is 6.2 percent, and the weight is 250 kilograms) is discharged from a discharge hole at the lower part of the cation exchange resin equipment and is put into a waste hydrochloric acid storage tank.
2. The waste hydrochloric acid raw material enters an activated carbon adsorption process at the flow rate of 6BV/h, the solution is circularly filtered in the activated carbon, the retention time is kept at 5min, and then the material is discharged through the activated carbon adsorption process.
3. The liquid absorbed by the active carbon is introduced into a feed inlet of a nanofiltration recovery processing device at the flow rate of 7 BV/h.
4. The frequency of a booster pump passing through the device is adjusted to 25Hz, and the liquid is conveyed to the nanofiltration recovery process at the flow rate of 8 BV/h.
5. The internal treatment pressure in the nanofiltration recovery process is increased to 5MPa, and the filtered acid liquor is discharged at the flow rate of 8BV/h through equipment.
6. The filtered acid solution is conveyed to an acid blending tank by a pump and is blended into an acid solution with a certain concentration and then is reused for the regeneration of the cation exchange resin.
The test method is as follows:
1. acid concentration test: and (3) performing acid-base titration, namely taking a 2mL acid solution sample of a standard solution NaOH (1mol/L), adding a drop of methyl orange indicator, performing base titration until the color of methyl red changes, and calculating to obtain the concentration of hydrochloric acid.
2. NMMO concentration test: high Performance Liquid Chromatography (HPLC) test comprises adjusting pH of sample solution to about 7, making mobile phase be 10mmol/L methanol water solution, setting wavelength of ultraviolet detector 205nm, sampling amount to 20 μ L, and quantifying by external standard method.
3. And (3) testing the chromaticity: the color of the samples taken from each fraction was measured according to the method of GB 11903-1989.
In the embodiment, the content of the NMMO solvent in the washing waste acid of the strong acid type uniform particle cation exchange resin is 6.2%, the concentration of hydrochloric acid is 4.8%, the chromaticity of the waste hydrochloric acid solution is obviously reduced after the waste hydrochloric acid solution is subjected to activated carbon adsorption treatment, the feeding amount in the nanofiltration recovery process is 5 BV/h-6 BV/h, the system pressure is kept at 4MPa, the system pressure fluctuates along with the increase of the feeding circulation amount, tests show that the hydrochloric acid in the treated permeation solution is completely recovered by 100%, the recovery rate of the NMMO solvent is 91.7%, the feeding amount of the system is 250kg of waste hydrochloric acid solution, the weight of the collected permeation solution is 225.1kg through nanofiltration, and the sewage discharge amount is effectively reduced by 90%.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (4)
1. A method for recovering N-methylmorpholine oxide solvent in Lyocell fiber regenerated acid is characterized by comprising the following steps:
collecting the Lyocell fiber regenerated acid as a waste hydrochloric acid solution;
the waste hydrochloric acid solution is treated by active carbon adsorption to obtain a first intermediate product, wherein,
the flow rate of the waste hydrochloric acid solution ranges from 3BV/h to 7 BV/h;
the retention time of the waste hydrochloric acid solution in the activated carbon adsorption treatment system is within a value range of 3-5 min;
carrying out nanofiltration treatment on the first intermediate product to obtain a recovered N-methylmorpholine oxide solvent;
in the nanofiltration treatment process, the intercepted concentrated solution is led to a sewage treatment system for sewage treatment, and the intermediate permeate liquid after nanofiltration is recycled for nanofiltration treatment until the final hydrochloric acid permeate liquid containing the N-methylmorpholine oxide solvent is discharged, so that the recovered N-methylmorpholine oxide solvent is obtained; in the process of obtaining the recovered N-methylmorpholine oxide solvent by the nanofiltration treatment of the first intermediate product,
The flow rate of the first intermediate product ranges from 4BV/h to 8 BV/h;
the value range of the process pressure in the nanofiltration treatment process is 3MPa to 7 MPa;
the flow rate of the intermediate permeate and the final permeate ranges from 2BV/h to 7 BV/h.
2. The method for recovering N-methylmorpholine oxide solvent from Lyocell fiber regenerating acid according to claim 1,
and in the nanofiltration treatment process, the first intermediate product enters a nanofiltration treatment system in a pump conveying mode.
3. The method for recovering N-methylmorpholine oxide solvent from Lyocell fiber regenerating acid according to claim 1,
the active carbon is powder active carbon with holes,
the activated carbon is uniformly filled in the activated carbon treatment system.
4. A preparation method of N-methylmorpholine oxide solvent is characterized by comprising the following steps:
blending the N-methylmorpholine oxide solvent recovered by the method of any one of claims 1 to 3 with hydrochloric acid to obtain the N-methylmorpholine oxide solvent with the concentration of hydrochloric acid suitable for cation regeneration.
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