CN114053746A - Method for recycling iron ions and sodium ions in vinyl chloride high-boiling residues - Google Patents

Method for recycling iron ions and sodium ions in vinyl chloride high-boiling residues Download PDF

Info

Publication number
CN114053746A
CN114053746A CN202010764567.1A CN202010764567A CN114053746A CN 114053746 A CN114053746 A CN 114053746A CN 202010764567 A CN202010764567 A CN 202010764567A CN 114053746 A CN114053746 A CN 114053746A
Authority
CN
China
Prior art keywords
ions
vinyl chloride
tower
sodium ions
iron ions
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.)
Granted
Application number
CN202010764567.1A
Other languages
Chinese (zh)
Other versions
CN114053746B (en
Inventor
董凌云
郭岩峰
曹树东
张辉
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
China Petroleum and Chemical Corp
Qilu Petrochemical Co of Sinopec
Original Assignee
China Petroleum and Chemical Corp
Qilu Petrochemical Co of Sinopec
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by China Petroleum and Chemical Corp, Qilu Petrochemical Co of Sinopec filed Critical China Petroleum and Chemical Corp
Priority to CN202010764567.1A priority Critical patent/CN114053746B/en
Publication of CN114053746A publication Critical patent/CN114053746A/en
Application granted granted Critical
Publication of CN114053746B publication Critical patent/CN114053746B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/10—Vacuum distillation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/42—Regulation; Control
    • B01D3/4211—Regulation; Control of columns
    • B01D3/4216—Head stream
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D3/00—Halides of sodium, potassium or alkali metals in general
    • C01D3/04—Chlorides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/10—Halides
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23J—REMOVAL OR TREATMENT OF COMBUSTION PRODUCTS OR COMBUSTION RESIDUES; FLUES 
    • F23J7/00—Arrangement of devices for supplying chemicals to fire

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

A method for recycling iron ions and sodium ions in vinyl chloride high boiling residues belongs to the technical field of recycling of vinyl chloride high boiling residues. The method comprises the following steps: 1) carrying out reduced pressure distillation on the chloroethylene high-boiling residue; after the reduced pressure distillation is finished, tower bottom components and tower top distillate oil are obtained; 2) adding the tower bottom components into an organic solvent, and fully combusting to obtain solid particles. The process conditions of reduced pressure distillation are as follows: the vacuum degree is 0.06-0.097 Mpa, and the tower top temperature is 50-99 ℃. The specific operation of the sufficient combustion in the step 2) is as follows: burning for 4-6 hours at 452-495 ℃. And 2) the organic solvent is tetrahydrofuran. The method for recycling the iron ions and the sodium ions in the vinyl chloride high-boiling residues has high removal rate of the iron ions and the sodium ions, and distillate oil at the top of the tower, the iron ions and the sodium ions can be recycled.

Description

Method for recycling iron ions and sodium ions in vinyl chloride high-boiling residues
Technical Field
A method for recycling iron ions and sodium ions in vinyl chloride high boiling residues belongs to the technical field of recycling of vinyl chloride high boiling residues.
Background
The chloroethylene high-boiling-point substance is a mixture generated in a high-boiling tower in the rectification process of chloroethylene, is a black-brown turbid liquid, has the colloid content of about 1-10wt%, contains various chlorides such as trichloromethane, dichloroethane, chlorohydrin, trichloroethane, dichloropropane, dichlorobutadiene, dichlorobutene, chlorobenzene, trichloropropene, tetrachlorobutane, dichlorocyclobutane, hexachlorohexadiene, chloroethylbenzene, chloropropylene ether, naphthalene, chlorobutenylbenzene, nitrogen-containing heterocyclic substances, acrylic resin, asphalt resin and the like, and has very complicated components. The vinyl chloride high boiling substance contains about 200 to 3000ppm of iron ions and about 30 to 500ppm of sodium ions. In the existing large-scale industrial production, a method of burning vinyl chloride high-boiling-point substances at 1200 ℃ by an industrial device, then cooling, and finally absorbing with water to obtain industrial hydrochloric acid is adopted to recycle the vinyl chloride high-boiling-point substances. The problem that prior art exists is that the heat exchange tube of the quencher in the industrial device frequently blocks up, mainly because the deposit scale deposit of sodium chloride and ferroferric oxide and iron sesquioxide and ferric chloride cause, must stop the vehicle and carry out manual scale removal every 10~15 days to cause huge manpower and materials and energy consumption, make the factory operating personnel to be bitter. Secondly, the obtained hydrochloric acid has yellow color and low quality, which is mainly caused by the existence of iron ions.
In order to solve the above problems, a process for removing and recycling iron ions and sodium ions in vinyl chloride high boiling residues needs to be explored. In the prior art, the processes of resin exchange and water washing are adopted for removing iron ions and sodium ions, but the resin exchange process is not feasible because vinyl chloride high-boiling residues contain 1-10wt% of colloid, and the colloid is easy to block micropores of the resin to inactivate the resin, so that the resin cannot be recycled. In addition, the water washing process also has the environmental protection problems of low conversion rate, waste water and waste residue treatment and the like. The metal ions are generally recovered by extraction, combustion and other methods.
Patent CN110395780A discloses a method for treating organic waste liquid containing phosphorus, iron and chlorine, comprising: 1) separating organic chloride in the organic waste liquid by adopting reduced pressure distillation to obtain organic chloride and a first residue; 2) carrying out reduced pressure rectification on the organic chloride, separating to obtain a crude product and a second residue, conveying the second residue to an incineration system, and absorbing hydrogen chloride in incineration tail gas to prepare hydrochloric acid; extracting the first residue to obtain an iron-containing product and a residual waste material; 3) purifying and concentrating the iron-containing product to obtain a ferric salt water treatment agent and hydrochloric acid; and distilling the residual waste to obtain hydrogen chloride and waste residues, recovering the hydrogen chloride to prepare hydrochloric acid, and conveying the waste residues to an incineration system. The disadvantages are as follows: firstly, the CN110395780A patent can generate waste liquid and waste residue which are difficult to treat, not beneficial to environmental protection and difficult to apply to industrial production, the material temperature of the second patent CN110395780A in the first step of reduced pressure distillation operation is 110-150 ℃, the vacuum degree of the system is controlled to be less than or equal to 1.0 KPa, the process conditions are very harsh, and the process is difficult to implement.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the method overcomes the defects of the prior art, and provides the method for recycling the iron ions and the sodium ions in the vinyl chloride high-boiling residues.
The technical scheme of the method for solving the technical problems is as follows: a method for recycling iron ions and sodium ions in vinyl chloride high-boiling residues comprises the following steps:
1) carrying out reduced pressure distillation on the chloroethylene high-boiling residue; after the reduced pressure distillation is finished, tower bottom components and tower top distillate oil are obtained;
2) adding the tower bottom components into an organic solvent, and fully combusting to obtain solid particles.
The process conditions of the reduced pressure distillation in the step 1) are as follows: vacuum degree of 0.06-0.097 Mpa, and tower top temperature (abbreviated as T)Top roof）50~99℃。
The specific operation of the sufficient combustion in the step 2) is as follows: burning for 4-6 hours at 452-495 ℃.
And 2) the organic solvent is tetrahydrofuran.
The organic solvent in the step 2) accounts for 4-6% of the mass of the components in the tower kettle.
The organic solvent in the step 2) accounts for 5-5.5% of the mass of the components in the tower kettle.
The distillate oil at the top of the tower in the step 1) accounts for 83-85% of the mass of the chloroethylene high-boiling residue.
The iron ion content in the distillate oil at the top of the tower in the step 1) is less than or equal to 3 ppm.
Further comprising a step 3), the specific operation of the step 3) is as follows: and adding the solid particles into a hydrochloric acid aqueous solution, stirring and mixing, crystallizing, and drying to obtain ferric chloride and sodium chloride.
And 3) the mass percentage concentration of the hydrochloric acid aqueous solution is 10-30%.
The invention is described below:
the applicant finds in research that the existing water washing method has a problem of high conversion rate due to the concentration of impurity metal ions in the high-boiling residues of vinyl chloride, and also has an environmental problem of waste water and waste residue treatment. The invention can control the content of impurity metal ions in the distillation fraction at the top of the tower by only controlling the temperature and the operating pressure at the top of the tower, so that the higher the content of iron ions and sodium ions in the raw materials of the chloroethylene high-boiling residue, the greater the advantages of the invention. Therefore, the content of iron ions in the vinyl chloride high boiling substance is preferably not less than 500ppm and the content of sodium ions is not less than 50 ppm. The invention realizes the separate treatment of the light fraction and the heavy fraction, namely, most of the light fraction is discharged from the top of the tower, and a small part of the heavy fraction is discharged from the bottom of the tower, and the heavy fraction can be used for producing ferric chloride and sodium chloride after organic matters such as colloid and the like are removed through proper treatment, thereby achieving the operation mode of circular economy, avoiding the problem of waste water and waste residue, and further solving the smoothness of a production back path.
The applicant considers that the vinyl chloride high-boiling residue contains 1-10wt% of colloid, has high boiling point and strong adhesion, fully utilizes the characteristic of large boiling point difference among components in the vinyl chloride high-boiling residue, and controls the temperature of the tower top to be 50-99 ℃, thereby ensuring that the distillate oil at the tower top only contains trace iron ions and hardly contains sodium ions (the content of the iron ions is less than or equal to 3ppm, and the content of the sodium ions is 0 ppm).
The process for removing and recycling the iron ions and the sodium ions in the vinyl chloride high-boiling residues is to remove and recycle the iron ions and the sodium ions in the vinyl chloride high-boiling residues under the process condition of reduced pressure distillation. At N =5 (lump), vacuum = 0.06-0.097 MPa, TTop roof= 50-99 ℃ and R = 0.2-1 (N represents the number of theoretical plates, TTop roofRepresenting the temperature at the top of the tower, and R representing the reflux ratio), obtaining colorless or light yellow top distillate oil with the weight percent of about 80-85 percent at the top of the tower, wherein the content of iron ions is less than or equal to 3ppm, and the content of sodium ions is 0 ppm; the distillation cut at the bottom of the tower is mainly a combination of colloid, iron ions, sodium ions and the like, and 5wt% of tetrahydrofuran is added after the distillation cut is discharged from the bottom of the tower, so that organic matters such as colloid can be dissolved, the fluidity of the colloid is improved (the colloid without 5wt% of tetrahydrofuran is poor in fluidity, insufficient in combustion, incomplete in combustion, prolonged in combustion time and not beneficial to the acidification treatment of inorganic matters in the next step), inorganic matters such as ferric chloride and sodium chloride can be dissolved, the organic matters such as colloid can be combusted more completely, the combustion time is obviously shortened, and the two purposes can be achieved. The organic matters such as colloid (nitrogenous heterocyclic substances, acrylic resin, asphalt resin and the like) and the like can be combusted more completely at the temperature of 450-500 ℃, and after the organic matters are completely removed, the solid particles obtained in the step 2) are inorganic salts or metal compounds (the main components are NaCl and FeeCl)3、Fe2O3) The method is used for producing ferric chloride and sodium chloride after being treated by the hydrochloric acid aqueous solution, realizes the operation mode of circular economy, and realizes the recycling of iron ions and sodium ions.
Compared with the prior art, the invention has the beneficial effects that:
1. the method has high removal rate of iron ions and sodium ions, and distillate oil on the top of the tower, the iron ions and the sodium ions can be recycled.
The present invention considers that vinyl chloride high boiling substance contains 1-10wt% of colloid, has high boiling point and strong adhesion, and completely removes the colloid by utilizing the characteristic of large boiling point difference of the substancesAnd recycling iron ions and sodium ions in the vinyl chloride high-boiling residues; firstly, the invention makes full use of the difference of boiling points among different components of the vinyl chloride high-boiling residue, and the light fraction and the heavy fraction are respectively treated, but not combusted together; most of the light fraction is discharged from the top of the column, and a small part of the heavy fraction is discharged from the bottom of the column. The tower top distillate oil is light distillate, contains trace impurity ions and can be used as chemical raw materials or enter an incinerator for combustion, economic benefits can be obtained if the tower top distillate oil is used as the chemical raw materials, heat energy can be provided if the tower top distillate oil enters the incinerator for combustion, a heat exchange tube of a quencher is not easy to scale and block, and long-period stable operation of the incinerator can be ensured; the bottom components are heavy fractions containing gum and iron and sodium ions which are separately discharged from the bottom of the column and are treated separately. Secondly, the discharged colloid and impurity ions are combusted in a reasonable temperature range (450-. The obtained solid particles are inorganic salt or metal compound (NaCl, FeCl)3、Fe2O3Etc.) by treatment with an aqueous hydrochloric acid solution to give Fecl3And the NaCl solution is used for producing ferric chloride and sodium chloride, so that the circular economy running mode is realized, and the recycling of iron ions and sodium ions is realized.
2. The method of the invention provides a method for removing and recycling iron ions and sodium ions in vinyl chloride high boiling residues, so that the contents of the iron ions and the sodium ions in the vinyl chloride high boiling residues are greatly reduced. The problem is solved from the production source, and obstacles are cleared for the smooth operation of a subsequent incineration device so as to ensure the long-period stable operation of the incinerator; the problem of condenser blockage is solved, the quality of hydrochloric acid is improved (the content of iron ions is reduced), and therefore the manpower, material and energy consumption of operators is reduced, and the circular economy running mode is realized.
3. The method is economic and environment-friendly, and no waste liquid or waste residue is generated. The iron ion content of the top distillate oil obtained in the step 1) is only 1-2.8 ppm, sodium ions are not contained, and the top distillate oil can be used as a chemical raw material or enter an incinerator for combustion, so that economic benefit is obtained. And 2) ferric chloride and sodium chloride can be obtained in the step 2) and can be used as chemical raw materials to obtain economic benefits. Meanwhile, the influence on the environment is reduced, the utilization rate of resources is improved, and considerable economic benefits are brought.
Detailed Description
The present invention is further illustrated by the following specific examples, of which example 1 is the most preferred.
Example 1
1) At N =5 (block), vacuum =0.08 MPa, TTop roofUnder the process conditions of =85 ℃ and R =0.3, vinyl chloride high boiling residue with iron ion content of 1000ppm and sodium ion content of 50ppm is added into a distillation tower for reduced pressure distillation; after the reduced pressure distillation is finished, obtaining tower kettle components at the tower kettle, and obtaining 83wt% of tower top distillate oil at the tower top; the iron ion content in the distillate oil at the top of the tower is 1ppm, and the sodium ion content is 0 ppm;
2) adding 5wt% of tetrahydrofuran into the components in the tower kettle, and fully combusting at 452 ℃ for 6 hours to obtain solid particles;
3) and adding 20% hydrochloric acid aqueous solution into the solid particles, stirring and mixing, crystallizing, and drying to obtain ferric chloride and sodium chloride.
Example 2
1) At N =5 (block), vacuum =0.076MPa, TTop roofUnder the process conditions of 75 ℃ and R =0.4, adding vinyl chloride high-boiling-point substance with iron ion content of 2000ppm and sodium ion content of 80 ppm into a distillation tower for reduced pressure distillation; after the reduced pressure distillation is finished, obtaining tower kettle components at the tower kettle, and obtaining 84wt% of tower top distillate oil at the tower top, wherein the iron ion content is 1.5ppm, and the sodium ion content is 0 ppm;
2) adding 5wt% of tetrahydrofuran into the components in the tower kettle, and fully combusting at 473 ℃ for 4.8 hours to obtain solid particles;
3) and adding a hydrochloric acid aqueous solution into the solid particles, stirring and mixing, crystallizing, and drying to obtain ferric chloride and sodium chloride.
Example 3
1) At N =5 (block), vacuum =0.09 MPa, TTop roofUnder the process conditions of temperature of 80 ℃ and R =0.6, the method comprises the following stepsAdding the chloroethylene high-boiling residue with iron ion content of 3000ppm and sodium ion content of 150 ppm into a distillation tower for reduced pressure distillation; after the reduced pressure distillation is finished, obtaining tower kettle components at the tower kettle, and obtaining 84.3wt% of tower top distillate oil at the tower top, wherein the iron ion content is 2.8ppm, and the sodium ion content is 0 ppm;
2) adding 5wt% of tetrahydrofuran into the components in the tower kettle, and fully combusting at 495 ℃ for 4 hours to obtain solid particles;
3) and adding a 15% hydrochloric acid aqueous solution into the solid particles, stirring and mixing, crystallizing, and drying to obtain ferric chloride and sodium chloride.
Example 4
1) At N =5 (lump), vacuum =0.06MPa, TTop roofUnder the process conditions of temperature of =90 ℃ and R =0.3, vinyl chloride high boiling residue with iron ion content of 2770ppm and sodium ion content of 50ppm is added into a distillation tower for reduced pressure distillation; after the reduced pressure distillation is finished, tower kettle components are obtained at the tower kettle, and 83.7wt% of tower top distillate oil is obtained at the tower top; the iron ion content in the distillate oil at the top of the tower is 1.9ppm, and the sodium ion content is 0 ppm;
2) adding 5.5wt% of tetrahydrofuran into the tower kettle components, and fully combusting at 460 ℃ for 5.8 hours to obtain solid particles;
3) and adding 30% hydrochloric acid aqueous solution into the solid particles, stirring and mixing, crystallizing, and drying to obtain ferric chloride and sodium chloride.
Example 5
1) At N =5 (block), vacuum =0.065 MPa, TTop roofUnder the process conditions of =99 ℃ and R =0.4, vinyl chloride high boiling residue with the iron ion content of 1850ppm and the sodium ion content of 80 ppm is added into a distillation tower for vacuum distillation; after the reduced pressure distillation is finished, obtaining tower kettle components at the tower kettle, and obtaining 84.8wt% of tower top distillate oil at the tower top, wherein the iron ion content is 1.3ppm, and the sodium ion content is 0 ppm;
2) adding 4wt% of tetrahydrofuran into the components in the tower kettle, and fully combusting at 485 ℃ for 5.2 hours to obtain solid particles;
3) and adding 20% hydrochloric acid aqueous solution into the solid particles, stirring and mixing, crystallizing, and drying to obtain ferric chloride and sodium chloride.
Example 6
1）At N =5 (block), vacuum =0.097 MPa, TTop roofUnder the process conditions of 50 ℃ and R =0.6, vinyl chloride high boiling residue with the iron ion content of 3300ppm and the sodium ion content of 150 ppm is added into a distillation tower for reduced pressure distillation; after the reduced pressure distillation is finished, obtaining tower kettle components at the tower kettle, and obtaining 84.2wt% of tower top distillate oil at the tower top, wherein the iron ion content is 2.2ppm, and the sodium ion content is 0 ppm;
2) adding the tower bottom components into 6wt% of tetrahydrofuran, and fully combusting at 470 ℃ for 4.8 hours to obtain solid particles;
3) and adding 10% hydrochloric acid aqueous solution into the solid particles, stirring and mixing, crystallizing, and drying to obtain ferric chloride and sodium chloride.
Comparative example 1
This comparative example is identical to example 1, except that no tetrahydrofuran is added in step 2).
Comparative example 2
This comparative example is identical to example 1, except that no tetrahydrofuran is added in step 2).
Comparative example 3
This comparative example is identical to example 1, except that no tetrahydrofuran is added in step 2).
Performance testing
The time spent in burning, the iron ion content in the overhead distillate, and the sodium ion content in the overhead distillate of step 2) of the examples and comparative examples are recorded and reported in table 1.
Table 1 results of performance testing of examples
Figure 273800DEST_PATH_IMAGE001
。
Table 2 comparative example performance test results
Figure DEST_PATH_IMAGE002
。
As can be seen from tables 1-2:
in the embodiment 1-6, the distillate oil obtained in the step 1) does not contain sodium ions, the content of iron ions is 1-2.8 ppm, the content is extremely low, and the distillate oil at the top of the tower can be used as a chemical raw material or can enter an incinerator for combustion, so that economic benefit is obtained. In the embodiment 1-6, the step 2) can obtain ferric chloride and sodium chloride which are used as chemical raw materials to obtain economic benefits.
After the tetrahydrofuran is added in the step 2) of the examples 1-3, the combustion time is obviously shorter than that of the comparative examples 1-3. The addition of tetrahydrofuran proves that the production efficiency of the method is obviously improved.
The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.

Claims (10)

1. A method for recycling iron ions and sodium ions in a vinyl chloride high-boiling residue is characterized by comprising the following steps:
1) carrying out reduced pressure distillation on the chloroethylene high-boiling residue; after the reduced pressure distillation is finished, tower bottom components and tower top distillate oil are obtained;
2) adding the tower bottom components into an organic solvent, and fully combusting to obtain solid particles.
2. The method for recycling iron ions and sodium ions in vinyl chloride high boiling residues as claimed in claim 1, wherein the method comprises the following steps: the process conditions of the reduced pressure distillation in the step 1) are as follows: the vacuum degree is 0.06-0.097 Mpa, and the tower top temperature is 50-99 ℃.
3. The method for recycling iron ions and sodium ions in vinyl chloride high boiling residues as claimed in claim 1, wherein the method comprises the following steps: the specific operation of the sufficient combustion in the step 2) is as follows: burning for 4-6 hours at 452-495 ℃.
4. The method for recycling iron ions and sodium ions in vinyl chloride high boiling residues as claimed in claim 1, wherein the method comprises the following steps: and 2) the organic solvent is tetrahydrofuran.
5. The method for recycling iron ions and sodium ions in vinyl chloride high boiling residues as claimed in claim 1, wherein the method comprises the following steps: and 2) the organic solvent accounts for 4-6% of the mass of the components in the tower kettle.
6. The method for recycling iron ions and sodium ions in vinyl chloride high boiling residues as claimed in claim 1 or 5, wherein: the organic solvent in the step 2) accounts for 5-5.5% of the mass of the components in the tower kettle.
7. The method for recycling iron ions and sodium ions in vinyl chloride high boiling residues as claimed in claim 1, wherein the method comprises the following steps: the distillate oil at the top of the tower in the step 1) accounts for 83-85% of the mass of the chloroethylene high-boiling residue.
8. The method for recycling iron ions and sodium ions in vinyl chloride high boiling residues as claimed in claim 1, wherein the method comprises the following steps: the iron ion content in the distillate oil at the top of the tower in the step 1) is less than or equal to 3 ppm.
9. The method for recycling iron ions and sodium ions in vinyl chloride high boiling residues as claimed in claim 1, wherein the method comprises the following steps: further comprising a step 3), the specific operation of the step 3) is as follows: and adding the solid particles into a hydrochloric acid aqueous solution, stirring and mixing, crystallizing, and drying to obtain ferric chloride and sodium chloride.
10. The method for recycling iron ions and sodium ions in vinyl chloride high boiling residues as claimed in claim 9, wherein the method comprises the following steps: and 3) the mass percentage concentration of the hydrochloric acid aqueous solution is 10-30%.
CN202010764567.1A 2020-08-03 2020-08-03 Method for recycling iron ions and sodium ions in vinyl chloride high-boiling residues Active CN114053746B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010764567.1A CN114053746B (en) 2020-08-03 2020-08-03 Method for recycling iron ions and sodium ions in vinyl chloride high-boiling residues

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010764567.1A CN114053746B (en) 2020-08-03 2020-08-03 Method for recycling iron ions and sodium ions in vinyl chloride high-boiling residues

Publications (2)

Publication Number Publication Date
CN114053746A true CN114053746A (en) 2022-02-18
CN114053746B CN114053746B (en) 2022-12-27

Family

ID=80231333

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010764567.1A Active CN114053746B (en) 2020-08-03 2020-08-03 Method for recycling iron ions and sodium ions in vinyl chloride high-boiling residues

Country Status (1)

Country Link
CN (1) CN114053746B (en)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0722758A2 (en) * 1995-01-20 1996-07-24 Air Products And Chemicals, Inc. Separation of fluid mixtures in multiple distillation columns
CN109970683A (en) * 2017-12-28 2019-07-05 中国石油化工股份有限公司 The separation method of epoxychloropropane
CN110395780A (en) * 2019-07-16 2019-11-01 太仓中化环保化工有限公司 A kind of processing method of high phosphorous iron content chlorinated waste water

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0722758A2 (en) * 1995-01-20 1996-07-24 Air Products And Chemicals, Inc. Separation of fluid mixtures in multiple distillation columns
CN109970683A (en) * 2017-12-28 2019-07-05 中国石油化工股份有限公司 The separation method of epoxychloropropane
CN110395780A (en) * 2019-07-16 2019-11-01 太仓中化环保化工有限公司 A kind of processing method of high phosphorous iron content chlorinated waste water

Also Published As

Publication number Publication date
CN114053746B (en) 2022-12-27

Similar Documents

Publication Publication Date Title
US20190023585A1 (en) Method and apparatus for the recovery and deep treatment of polluted acid
CN109867296A (en) A kind of industrial chlorinations sodium waste salt dregs refining methd
CN102910757B (en) Treatment technique of waste water generated in production of o-nitrophenol
CN103803638B (en) Method for recycling waste mercury catalyst
CN102583849A (en) Treatment technique of tetrabromobisphenol A production wastewater
CN104192802B (en) The by-product hydrochloric acid purifying method of the chloro-6-fluorobenzaldehyde of 2-or analogue
CN106495404A (en) A kind of processing method of the high salinity cupric organic wastewater of highly acidity
CN106006681B (en) A kind of method of high slat-containing wastewater recycling treatment
CN111744922A (en) Fly ash treatment process in waste incineration process
CN103395925A (en) Treatment method for recycling para-hydroxybenzoic acid wastewater
CN106745416B (en) Application of arsenic and fluorine in high-temperature molten copper slag treatment of contaminated acid and application method thereof
CN104878201B (en) A kind of method of the recovering rare earth from RE waste water is contained
CN114053746B (en) Method for recycling iron ions and sodium ions in vinyl chloride high-boiling residues
CN103014338A (en) Method for processing poor organic phase after solvent extraction indium extracting
CN105543500B (en) The method that reclaims zinc is discarded in mud cake containing zinc from electrogalvanizing
CN110818569B (en) Treatment method of RT base production waste gas
CN101885657B (en) Method for recovering symmetrical straight-chain even normal paraffin from waste liquor
CN111498871A (en) System and method for treating waste salt residues mixed by sodium sulfate and sodium chloride
CN103819042B (en) A kind of hydrochloride waste purifying treatment method
CN110980847A (en) Treatment and recovery system and method for waste alkali in methane chloride production
CN103130296B (en) Acetate-containing industrial organic wastewater treatment process
NL2029939B1 (en) Treatment process for purifying chlorine-containing wastewater by crystallization of ammonium salt
CN106673067B (en) Utilize the method for waste sulfuric acid from alkylation production LITHIUM BATTERY manganese sulfate
CN108218075B (en) Method for recovering organic matters from waste liquid generated in production of methane chloride
CN115433841B (en) Method for recycling waste mercury catalyst

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant