CN106349124B - A kind of method for recycling organic and inorganic component in dimethyl sulfoxide (DMSO) abraum salt - Google Patents
A kind of method for recycling organic and inorganic component in dimethyl sulfoxide (DMSO) abraum salt Download PDFInfo
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- CN106349124B CN106349124B CN201610762445.2A CN201610762445A CN106349124B CN 106349124 B CN106349124 B CN 106349124B CN 201610762445 A CN201610762445 A CN 201610762445A CN 106349124 B CN106349124 B CN 106349124B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/42—Separation; Purification; Stabilisation; Use of additives
- C07C303/44—Separation; Purification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D9/00—Nitrates of sodium, potassium or alkali metals in general
- C01D9/16—Purification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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Abstract
The present invention proposes a kind of method for recycling organic and inorganic component in dimethyl sulfoxide (DMSO) abraum salt, specifically the DMSO industrial waste salts of hot melt are transferred to by conveyor in extraction equipment, it is stupid to be passed through extractant, benzene is mixed in the apparatus with abraum salt, extraction heat liquid after extraction saturation enters crystallisation by cooling slot, at 25 30 DEG C of room temperature centrifugation obtain MSM crystalline solid；The inorganic abraum salt of extraction leftover of extraction equipment discharge adds in 70 DEG C of hot water dissolving to saturated solution, is concentrated by evaporation, recrystallization obtains nitric acid sodium crystal after centrifugation.The technological process is simple, it is easier to implement, and the technique realizes separating and recovering for sodium nitrate and sodium methanesulfonate, can obtain nitric acid sodium crystal and sodium methanesulfonate that purity is up to more than 97%.
Description
Technical field
The invention belongs to dimethyl sulfoxide (DMSO)s to produce waste residue resource utilization technology field, and particularly one kind is by primary
Organic component and substep temperature control recrystallization separation sodium nitrate and sodium methanesulfonate in extraction recycling dimethyl sulfoxide waste residue
Method.
Background technology
1 ton of product is often produced in DMSO production processes and just generates 0.2 ton of abraum salt, wherein containing MSM and DMSO organic substances,
And the inorganic components such as sodium nitrate and sodium methanesulfonate, there is higher recovery value.
It can be turned waste into wealth by this item purpose implementing process, in the Heavy environmental pollution that elimination DMSO abraum salts may be brought
Meanwhile higher economic well-being of workers and staff is created to enterprise, meet the objective of Enterprise Circular Economy Green Development, solve to restrict dimethyl Asia
The bottleneck problem of sulfone production development.The project implementation has preferable social benefit and environmental benefit.
Invention content
The present invention by single extraction and is evaporated with regard to the organic component in recyclable DMSO abraum salts using a kind of extractant, and
The recrystallizing technology condition of a recrystallization separation sodium nitrate and sodium methanesulfonate is found out, there is preferable economic benefit.It should
Method is compared with " a kind of method of multitple extraction recycling DMSO abraum salts ", and flow is simpler, only with a kind of extractant benzene through primary extraction
The recycling extraction of organic component can be realized by taking, and be stirred without microwave, only stirred with conventional mechanical, be easier in engineering
Implement, and the technique realizes separating and recovering for sodium nitrate and sodium methanesulfonate, can obtain purity and be up to more than 97%
Nitric acid sodium crystal and sodium methanesulfonate.
Specifically comprise the following steps：
（1）The DMSO industrial waste salts of hot melt are transferred to by conveyor in extraction equipment, are passed through extractant benzene, benzene
It is mixed in the apparatus with abraum salt, mechanical agitation, temperature is maintained at 50 DEG C in extraction equipment；
（2）Extraction heat liquid after extraction saturation enters crystallisation by cooling slot, at 25-30 DEG C of room temperature centrifugation obtain MSM crystallizations
Body；
（3）Cold extract liquor after centrifugation enters fractionating device, and benzene vapour is steamed at 80 DEG C, and benzene vapour returns after cooling
With；And the semisolid mixture of obtained DMSO and MSM are fractionated, into the DMSO process for refining sections of original production device, after refining
Recycle product；
（4）The inorganic abraum salt of extraction leftover of extraction equipment discharge is poured into dissolving tank, adds in 70 DEG C of hot water dissolving extremely
Saturated solution, inorganic abraum salt is with adding the mass ratio of water to be less than 1：1, it is 7 to add nitric acid tune pH value；
（5）Saturated solution is pumped into heating and evaporating unit 1, concentration is evaporated at a temperature of 85-132 DEG C, when volume about
For original volume about 1/2 when, be pumped into recrystallization reactor 1 in, recrystallized at room temperature, obtained after centrifugation sodium nitrate crystalline substance
Body 1 and filtrate 1；
（6）Filtrate 1 enters heating and evaporating unit 2, after continuing to evaporate portion of water at a temperature of 85-132 DEG C, cooling
It is crystallized to 65-75 DEG C, centrifugation obtains the nitric acid sodium crystal of bottom and filtrate 2, filtrate 2 is released cooling, bottom crystal is
Sodium nitrate, supernatant liquid pour out thickening filtration and obtain pyrovinic acid sodium crystal, and filtered fluid may be incorporated into pending liquid and handle again.
Step（1）MSM contents 23% in middle DMSO industrial waste salts, DMSO contents 14%；The mass ratio of extractant benzene and abraum salt
It is 3.5：0.5-1.5.
Step（5）In, saturated solution is pumped into heating and evaporating unit 1, concentration is evaporated at a temperature of 120 DEG C, works as body
When product is about about the 1/2 of original volume, it is pumped into recrystallization reactor 1, is recrystallized at room temperature, nitric acid is obtained after centrifugation
Sodium crystal 1 and filtrate 1.
Step（6）In, filtrate 1 enters heating and evaporating unit 2, after continuing to evaporate portion of water at a temperature of 120 DEG C,
It cools to 70 DEG C to be crystallized, centrifugation obtains the nitric acid sodium crystal of bottom and filtrate 2, filtrate 2 is released cooling, bottom crystal is
Sodium nitrate, supernatant liquid pour out thickening filtration and obtain pyrovinic acid sodium crystal, and filtered fluid may be incorporated into pending liquid and handle again.
The present invention only directly continuously extracts the very high MSM crystalline solid of purity with a kind of extractant, and the rate of recovery is pure up to 95%
Degree is more than 99.7%, can be sold after simple drying-granulating directly as product.Sodium nitrate and pyrovinic acid can also be separated and recovered
Sodium.
Description of the drawings
Fig. 1 tests simulating lab test device for DMSO abraum salt organic components recovery process.
Fig. 2 is DMSO abraum salt recovery process flows.
Embodiment 1
With the experiment of following experimental provision simulation extraction and recovery MSM and DMSO in experiment.Experimental provision is by glycerol bath and adds
The compositions such as thermal and glass bar, beaker, thermometer, iron stand.See Fig. 1.
Implementation steps：
1）Industrial waste salt 10.3042g is taken, is extracted 5 times at 50 DEG C with 40mL benzene, is extracted postcooling every time to room temperature, wait to analyse
Crystal is filtered out after going out crystalline solid, collects the crystal obtained every time, after hair-dryer or baking oven drying removal benzene, MSM crystal claims
Weight 2.2515g, regathers in measuring cup, is put into spare in drier.The measure of crystal purity.Recycling in laboratory is obtained
A MSM crystal send to the factory laboratory and is analyzed, and has done parallel three times, MSM contents in measure crystal.Crystal purity is
99.73%, remaining 0.27% impurity is DMSO.
2）In 10.3042g abraum salts, through inorganic abraum salt 4.3576g is obtained by extraction, 42.3%, MSM of former abraum salt quality is accounted for
Crystal 2.2515g, the rate of recovery 95%.Crystal purity is 99.73%, remaining 0.27% impurity is DMSO.
Embodiment 2
The separating experiment of inorganic component in DMSO abraum salts.
1）The residual object of extraction after extraction is collected, is placed on that the remaining benzene of removal and moisture are dried in air dry oven.
It is called inorganic abraum salt.The inorganic abraum salts of 20g are weighed, are slowly added into 20mL water while stirring, solution system temperature in course of dissolution
It is substantially reduced, can add in promote temperature to room temperature slightly（25-30℃）, to accelerate solution rate.Most of salt dissolved with
Afterwards, it is filtered with sand core funnel, obtains filtrate.
2）On magnetic force heating stirrer, filtrate is heated to 120 DEG C and is evaporated concentration, when volume reduces about half
When, lift down to be put into carrying out crystallisation by cooling at room temperature from blender.After temperature drops to room temperature, then 40min is stood, filtered at this time
One layer of more white crystal has been precipitated in the bottom of liquid.
3）When observation filtrate does not have new crystal precipitation, filtrate at this time is filtered at normal temperatures with sand core funnel,
Nitric acid sodium crystal is obtained, is directly weighed as 4.5166g, it is 97.2% to measure the sodium nitrate purity in crystal.Remaining 2.8% be methyl
Sodium sulfonate.
4）By 3）In filtrate, again heat concentration condition it is the same, when being concentrated to volume half or so, crystal is arranged at bottom
It is precipitated, is filtered with the sand core funnel of heat at 70 DEG C, obtains nitric acid sodium crystal again, be directly weighed as 3.8450g, measure brilliant
Sodium nitrate purity in body is 97.4%.
5）4）Crystallization is precipitated in bottom again after middle filtrate cooling, and upper liquid has muddy fine crystals, pours out supernatant liquid
It carries out being concentrated to give pyrovinic acid sodium crystal, weigh about 2.5203g.Bottom crystal body is weighed as after blotting paper absorbs water
2.2501g。
Recrystallizer recycles nitric acid sodium crystal 10.6117g, the rate of recovery 82% in total three times, and the methanesulfonic sodium crystal rate of recovery is
43.2%。
The mineral waste salt quality that recrystallization is participated in Practical Project is more, and loss is relatively small, and can repeated recrystallize, then nitric acid
The rate of recovery of sodium and sodium methanesulfonate can be some higher.
Embodiment 3
Recycle MSM and DMSO techniques in DMSO abraum salts.
1）By DMSO industrial waste salts (MSM contents 23%, the DMSO contents 14% of hot melt）Extraction is transferred to by conveyor
It takes in device, the ratio of extractant benzene and abraum salt：Benzene（3.5m3）：Abraum salt（1 ton）.Benzene is mixed in the apparatus with abraum salt
Contact, mechanical agitation, temperature are maintained at 50 DEG C.
2）Extraction heat liquid after extraction saturation enters crystallisation by cooling slot, in room temperature（25-30℃）Lower centrifugation obtains MSM crystallizations
Body can obtain 0.22 ton of MSM, and the rate of recovery is 95% in laboratory, purity 99.73%.
3）Cold extract liquor after centrifugation enters fractionating device, and benzene vapour, benzene vapour reuse after cooling are steamed at 80 DEG C.
4）Into the DMSO process for refining sections of original production device, production is recycled after refining for the semisolid mixture of DMSO and MSM
Product.Can extract in practice it is multiple batches of after, redistillation go out benzene and recycling DMSO and MSM mixtures.
2. sodium nitrate and methanesulfonic sodium recovery purifying technique
5）It is the referred to as inorganic abraum salt of inorganic component by the extraction leftover of extraction equipment discharge, inorganic abraum salt 0.43 can be obtained
Ton, inorganic abraum salt is poured into dissolving tank, adds in 70 DEG C of hot water dissolving to saturated solution（Amount of water is less than 1:1）.Add nitric acid
It is 7 to adjust pH value.
6）Saturated solution is pumped into heating and evaporating unit 1, concentration is evaporated at a temperature of 120 DEG C.When volume is about original
Volume about 1/2 when, be pumped into recrystallization reactor 1 in, recrystallized at room temperature.Nitric acid sodium crystal 1 is obtained after centrifugation
With filtrate 1.
7）Filtrate 1 enters heating and evaporating unit 2, after continuing to evaporate portion of water at a temperature of 120 DEG C（Flowmeter control
System）, cool to 70 DEG C and crystallized, centrifugation while hot obtains the nitric acid sodium crystal of bottom and filtrate 2, and filtrate 2 is released cooling, bottom
Portion's crystallization is sodium nitrate, and supernatant liquid pours out thickening filtration and obtains pyrovinic acid sodium crystal, and filtered fluid may be incorporated into pending liquid
It handles again.
Claims (2)
- A kind of 1. method for recycling organic and inorganic component in dimethyl sulfoxide (DMSO) abraum salt, which is characterized in that include the following steps：（1）The DMSO industrial waste salts of hot melt are transferred to by conveyor in extraction equipment, are passed through extractant benzene, benzene is with giving up Salt is mixed in the apparatus, mechanical agitation, and temperature is maintained at 50 DEG C in extraction equipment, the DMSO industrial waste salts Middle MSM contents 23%, DMSO contents 14%, sodium nitrate and sodium methanesulfonate inorganic component；The mass ratio of extractant benzene and abraum salt is 3.5：0.5-1.5；（2）Extraction heat liquid after extraction saturation enters crystallisation by cooling slot, at 25-30 DEG C of room temperature centrifugation obtain MSM crystalline solid；（3）Cold extract liquor after centrifugation enters fractionating device, and benzene vapour, benzene vapour reuse after cooling are steamed at 80 DEG C；And The semisolid mixture of obtained DMSO and MSM are fractionated, into the DMSO process for refining sections of original production device, production is recycled after refining Product；（4）The inorganic abraum salt of extraction leftover of extraction equipment discharge is poured into dissolving tank, adds in 70 DEG C of hot water dissolving to saturation Solution, inorganic abraum salt is with adding the mass ratio of water to be less than 1：1, it is 7 to add nitric acid tune pH value；（5）Saturated solution is pumped into heating and evaporating unit 1, concentration is evaporated at a temperature of 120 DEG C, when volume is original volume When 1/2, it is pumped into recrystallization reactor 1, is recrystallized at room temperature, nitric acid sodium crystal 1 and filtrate 1 are obtained after centrifugation；（6）Filtrate 1 enters heating and evaporating unit 2, after continuing to evaporate portion of water at a temperature of 85-132 DEG C, cools to 65-75 DEG C is crystallized, and centrifugation obtains the nitric acid sodium crystal of bottom and filtrate 2, filtrate 2 is released cooling, bottom crystal is nitre Sour sodium, supernatant liquid pour out thickening filtration and obtain pyrovinic acid sodium crystal, and filtered fluid may be incorporated into pending liquid and handle again.
- 2. the method for organic and inorganic component in recycling dimethyl sulfoxide (DMSO) abraum salt described in claim 1, which is characterized in that step （6）In, filtrate 1 enter heating and evaporating unit 2, after continuing to evaporate portion of water at a temperature of 120 DEG C, cool to 70 DEG C into Row crystallization, centrifugation obtain the nitric acid sodium crystal of bottom and filtrate 2, and filtrate 2 released cooling, and bottom crystal is sodium nitrate, upper strata Liquid pouring goes out thickening filtration and obtains pyrovinic acid sodium crystal, and filtered fluid may be incorporated into pending liquid and handle again.
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Effective date of registration: 20190419 Address after: 408300 Tongji Village, Chengxi Town, Dinjiang County, Chongqing Patentee after: Chongqing Xingfa Jinguan Chemical Co. Ltd. Address before: 443711 Hunan Road, Gufu Town, Xingshan County, Yichang City, Hubei Province Patentee before: Hubei Xingfa Chemical Group Corp., Ltd. |
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