CN107602611A - A kind of production technology that hydroxy ethylene diphosphonic acid is prepared using chloroacetic chloride waste liquid - Google Patents
A kind of production technology that hydroxy ethylene diphosphonic acid is prepared using chloroacetic chloride waste liquid Download PDFInfo
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- CN107602611A CN107602611A CN201710809614.8A CN201710809614A CN107602611A CN 107602611 A CN107602611 A CN 107602611A CN 201710809614 A CN201710809614 A CN 201710809614A CN 107602611 A CN107602611 A CN 107602611A
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- chloroacetic chloride
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Abstract
The invention discloses a kind of production technology that hydroxy ethylene diphosphonic acid is prepared using chloroacetic chloride waste liquid, using chloroacetic chloride waste liquid, deionized water and the phosphorus trichloride that mass fraction is 50 70% as raw material, according to step in detail below, completes production technology；Active components of the HEDP produced by the invention in terms of HEDP is more than 98%；The isolated sterling acetum percentage composition of this technique is 70% 90%；The present invention has developed the technique that HEDP is prepared using chloroacetic chloride waste liquid, compared with traditional handicraft, improves the utilization ratio of chloroacetic chloride, realization is turned waste into wealth, and significantly reduces production cost.Pass through the present invention, being recycled for impure chloroacetic chloride is realized, the purity of byproduct acetic acid is higher, economizes on resources, the yield of " three wastes " during polyisobutylene phosphate production is greatly reduced, the HEDP product indexs of preparation meet industrial products index.
Description
Technical field
The present invention relates to a kind of production technology of hydroxy ethylene diphosphonic acid, and in particular to one kind utilizes chloroacetic chloride waste liquid system
The production technology of standby hydroxy ethylene diphosphonic acid.
Background technology
Polyisobutylene phosphate be integrate scale inhibition, scattered, inhibition, etc. multiple performance water treatment agent, before
Scape is extensive.Its with special nature so as in industrial circulation water treatment, oil-field flooding, mesohigh boiler with special use
On the way.Existing to produce a large amount of chloroacetic chloride waste liquids on the phosphatic preparation technology of polyisobutylene, waste liquid key component is chloroacetic chloride
And acetic acid, contain less amount of aceticanhydride and butanone.Because chloroacetic chloride and butanone boiling point are closer to, it is difficult to separating-purifying, also difficulty is entered
Row biochemical treatment is discharged, and can cause the great wasting of resources.Therefore, the recycling of this chloroacetic chloride waste liquid is developed, no
The utilization ratio of chloroacetic chloride is improve only, expands economic benefit, and waste liquid generation can be reduced.
Hydroxy ethylene diphosphonic acid（HEDP）It is a kind of organophosphor acids anti-incrustation corrosion inhibitor, frequently as metal and nonmetallic
Cleaning agent, anti-incrustation corrosion inhibitor, application field are wide.Therefore the above-mentioned chloroacetic chloride waste liquid of development utilization prepare HEDP production technology into
For research emphasis.
The content of the invention
It is difficult to back in view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to now provide a kind of chloroacetic chloride waste liquid that effectively solves
The drawbacks of receiving processing, improves the utilization ratio of chloroacetic chloride, production cost is greatly reduced, turn waste into wealth, developed resource-conserving
The production technology that hydroxy ethylene diphosphonic acid is prepared using chloroacetic chloride waste liquid.
In order to solve the above technical problems, the technical solution adopted by the present invention is：One kind prepares hydroxyl using chloroacetic chloride waste liquid
The production technology of ethylidene diphosphonic acid, its innovative point are：Using mass fraction as 50-70% chloroacetic chloride waste liquid, deionized water and
Phosphorus trichloride is raw material, according to step in detail below, completes production technology；It is described to comprise the following steps that：
（1）Thoroughly cleaning reactor, check valve, pressure；
（2）1000 parts by weight chloroacetic chloride waste liquids are pumped into reactor bottom, open stirring；
（3）Deionized water 150-450 parts by weight are slowly added dropwise, 10-50 DEG C of temperature control during dropwise addition, after completion of dropwise addition, stirring 2 is small
When；
Reaction equation：
；
（4）60-100 DEG C is continuously heating to, collects front-end volatiles 120-300 parts by weight, sewage plant is delivered to and carries out biochemical treatment；
（5）Distillation terminates, and obtains acetum, and feed liquid sample examination in reactor, the acetic acid content is 70-90%；
（6）ON cycle water, when material in reactor temperature is down to 30 DEG C, the parts by weight of phosphorus trichloride 1060 are slowly added dropwise, are added dropwise
Process temperature control is at 10-50 DEG C；
（7）After completion of dropwise addition, slowly heating esterification, when temperature rises to 105 DEG C, 1-4 hours are incubated；
Reaction equation：
；
（8）The hydrolysis of 300 parts by weight of deionized water, hydrolysis time 2 hours is slowly added dropwise；
（9）Distillation and dense time liquid reception device are opened, concentration distillation, receives acetum；
（10）Rush steaming to terminate, add 250-400 parts by weight of deionized water, stir；
（11）95 DEG C are cooled to, adds hydrogen peroxide for decoloration, is discharged, is examined.
Further, the step（2）In chloroacetic chloride waste liquid be containing acetic acid, butanone, aceticanhydride impurity chloroacetic chloride, it is described
Chloroacetic chloride accounts for the 50-70% of waste liquid gross mass, and the acetic acid accounts for the 20-30% of waste liquid gross mass, and the butanone accounts for waste liquid gross mass
2-6%, the aceticanhydride accounts for the 2-12% of waste liquid gross mass.
Beneficial effects of the present invention are as follows：Active components of the HEDP produced by the invention in terms of HEDP is more than 98%；This work
The isolated sterling acetum percentage composition of skill is 70%-90%；The present invention has developed prepares HEDP using chloroacetic chloride waste liquid
Technique, compared with traditional handicraft, improve the utilization ratio of chloroacetic chloride, realization is turned waste into wealth, and significantly reduces production cost.
By the present invention, being recycled for impure chloroacetic chloride is realized, the purity of byproduct acetic acid is higher, economizes on resources, greatly
The yield for reducing " three wastes " during polyisobutylene phosphate production, the HEDP product indexs of preparation meet industrial production
Product index.
Brief description of the drawings
Fig. 1 is the process chart of the present invention.
Embodiment
Embodiments of the present invention are illustrated by particular specific embodiment below, those skilled in the art can be by this explanation
Content disclosed by book understands other advantages and effect of the present invention easily.
It is as shown in Figure 1 the process chart of the present invention；
Embodiment 1
A kind of production technology that hydroxy ethylene diphosphonic acid is prepared using chloroacetic chloride waste liquid, using mass fraction as 50% chloroacetic chloride
Waste liquid, deionized water and phosphorus trichloride are raw material, according to step in detail below, complete production technology；Comprise the following steps that：
（1）Thoroughly cleaning reactor, check valve, pressure；
（2）1000 parts by weight chloroacetic chloride waste liquids are pumped into reactor bottom, open stirring, chloroacetic chloride waste liquid is containing acetic acid, butanone, vinegar
The chloroacetic chloride of acid anhydride impurity, chloroacetic chloride account for the 70% of waste liquid gross mass, and acetic acid accounts for the 20% of waste liquid gross mass, and butanone accounts for waste liquid gross mass
6%, aceticanhydride accounts for the 4% of waste liquid gross mass；
（3）The parts by weight of deionized water 200 are slowly added dropwise, 10 DEG C of temperature control during dropwise addition, after completion of dropwise addition, stir 2 hours；
Reaction equation：
；
（4）60 DEG C are continuously heating to, collects the parts by weight of front-end volatiles 120, sewage plant is delivered to and carries out biochemical treatment；
（5）Distillation terminates, and obtains acetum, feed liquid sample examination in reactor, acetic acid content 70%；
（6）ON cycle water, when material in reactor temperature is down to 30 DEG C, the parts by weight of phosphorus trichloride 1060 are slowly added dropwise, are added dropwise
Process temperature control is at 10 DEG C；
（7）After completion of dropwise addition, slowly heating esterification, when temperature rises to 105 DEG C, 1 hour is incubated；
Reaction equation：
；
（8）The hydrolysis of 300 parts by weight of deionized water, hydrolysis time 2 hours is slowly added dropwise；
（9）Distillation and dense time liquid reception device are opened, concentration distillation, receives acetum；
（10）Rush steaming to terminate, add 250 parts by weight of deionized water, stir；
（11）95 DEG C are cooled to, adds hydrogen peroxide for decoloration, is discharged, is examined.
Embodiment 2
A kind of production technology that hydroxy ethylene diphosphonic acid is prepared using chloroacetic chloride waste liquid, using mass fraction as 70% chloroacetic chloride
Waste liquid, deionized water and phosphorus trichloride are raw material, according to step in detail below, complete production technology；Comprise the following steps that：
（1）Thoroughly cleaning reactor, check valve, pressure；
（2）1000 parts by weight chloroacetic chloride waste liquids are pumped into reactor bottom, open stirring, chloroacetic chloride waste liquid is containing acetic acid, butanone, vinegar
The chloroacetic chloride of acid anhydride impurity, chloroacetic chloride account for the 52% of waste liquid gross mass, and acetic acid accounts for the 30% of waste liquid gross mass, and butanone accounts for waste liquid gross mass
6%, aceticanhydride accounts for the 12% of waste liquid gross mass；
（3）The parts by weight of deionized water 400 are slowly added dropwise, 50 DEG C of temperature control during dropwise addition, after completion of dropwise addition, stir 2 hours；
Reaction equation：
；
（4）100 DEG C are continuously heating to, collects the parts by weight of front-end volatiles 300, sewage plant is delivered to and carries out biochemical treatment；
（5）Distillation terminates, and obtains acetum, feed liquid sample examination in reactor, acetic acid content 90%；
（6）ON cycle water, when material in reactor temperature is down to 30 DEG C, the parts by weight of phosphorus trichloride 1060 are slowly added dropwise, are added dropwise
Process temperature control is at 50 DEG C；
（7）After completion of dropwise addition, slowly heating esterification, when temperature rises to 105 DEG C, 4 hours are incubated；
Reaction equation：
；
（8）The hydrolysis of 300 parts by weight of deionized water, hydrolysis time 2 hours is slowly added dropwise；
（9）Distillation and dense time liquid reception device are opened, concentration distillation, receives acetum；
（10）Rush steaming to terminate, add 400 parts by weight of deionized water, stir；
（11）95 DEG C are cooled to, adds hydrogen peroxide for decoloration, is discharged, is examined.
Embodiment 3
A kind of production technology that hydroxy ethylene diphosphonic acid is prepared using chloroacetic chloride waste liquid, using mass fraction as 60% chloroacetic chloride
Waste liquid, deionized water and phosphorus trichloride are raw material, according to step in detail below, complete production technology；Comprise the following steps that：
（1）Thoroughly cleaning reactor, check valve, pressure；
（2）1000 parts by weight chloroacetic chloride waste liquids are pumped into reactor bottom, open stirring, chloroacetic chloride waste liquid is containing acetic acid, butanone, vinegar
The chloroacetic chloride of acid anhydride impurity, chloroacetic chloride account for the 60% of waste liquid gross mass, and acetic acid accounts for the 28% of waste liquid gross mass, and butanone accounts for waste liquid gross mass
2%, aceticanhydride accounts for waste liquid gross mass 10%；
（3）The parts by weight of deionized water 300 are slowly added dropwise, 30 DEG C of temperature control during dropwise addition, after completion of dropwise addition, stir 2 hours；
Reaction equation：
；
（4）80 DEG C are continuously heating to, collects the parts by weight of front-end volatiles 210, sewage plant is delivered to and carries out biochemical treatment；
（5）Distillation terminates, and obtains acetum, feed liquid sample examination in reactor, acetic acid content 80%；
（6）ON cycle water, when material in reactor temperature is down to 30 DEG C, the parts by weight of phosphorus trichloride 1060 are slowly added dropwise, are added dropwise
Process temperature control is at 30 DEG C；
（7）After completion of dropwise addition, slowly heating esterification, when temperature rises to 105 DEG C, 3 hours are incubated；
Reaction equation：
；
（8）The hydrolysis of 300 parts by weight of deionized water, hydrolysis time 2 hours is slowly added dropwise；
（9）Distillation and dense time liquid reception device are opened, concentration distillation, receives acetum；
（10）Rush steaming to terminate, add 320 parts by weight of deionized water, stir；
（11）95 DEG C are cooled to, adds hydrogen peroxide for decoloration, is discharged, is examined.
Embodiment 4
A kind of production technology that hydroxy ethylene diphosphonic acid is prepared using chloroacetic chloride waste liquid, using mass fraction as 60% chloroacetic chloride
Waste liquid, deionized water and phosphorus trichloride are raw material, according to step in detail below, complete production technology；Comprise the following steps that：Thoroughly
Clean the relevant devices such as reactor, condenser, check valve, pressure；By 7880kg chloroacetic chloride waste liquids, GC detection butanone
4.8587%, chloroacetic chloride 51.0581%, acetic acid 33.0258%, aceticanhydride 7.2109%, reactor bottom is pumped into, opens stirring, condenser；
2500kg deionized waters are slowly added dropwise, temperature control is no more than 40 DEG C；After being added dropwise, 100 DEG C, in temperature-rise period are continuously heating to,
Front-end volatiles 1500kg is collected, sewage plant is delivered to and carries out biochemical treatment；Feed liquid sampling detection, acetic acid content 79.8% in reactor.Instead
Answer kettle interlayer ON cycle water to cool, when temperature is down to 20 DEG C, phosphorus trichloride 5300kg is slowly added dropwise, temperature is kept during dropwise addition
Degree is no more than 50 DEG C, completion of dropwise addition, slowly heating esterification, when temperature rises to 110 DEG C, insulation reaction 2 hours, is slowly added to
1500kg deionized waters, are hydrolyzed；After hydrolysis terminates, distillation and acetic acid reception device are opened, heating distillation, receives acetic acid；
After concentration terminates, start punching and steam, 125 DEG C of temperature control is following, rushes after steaming terminates, addition 4000kg water, stirs；It is cooled to 95
DEG C, hydrogen peroxide for decoloration is added, discharging, after testing, for the active quantities that product is counted using acid as 60.48%, other indexs meet industry
Product requirement.
Embodiment 5
A kind of production technology that hydroxy ethylene diphosphonic acid is prepared using chloroacetic chloride waste liquid, using mass fraction as 50% chloroacetic chloride
Waste liquid, deionized water and phosphorus trichloride are raw material, according to step in detail below, complete production technology；Comprise the following steps that：Thoroughly
Clean the relevant devices such as reactor, condenser, check valve, pressure；By 10000kg chloroacetic chloride waste liquids, GC detection butanone
4.4024%, chloroacetic chloride 64.3530%, acetic acid 25.213%, aceticanhydride 2.9531%, reactor bottom is pumped into, opens stirring, condenser；
2200kg deionized waters are slowly added dropwise, temperature control is no more than 40 DEG C；After being added dropwise, 110 DEG C, in temperature-rise period are continuously heating to,
Front-end volatiles 1450kg is collected, sewage plant is delivered to and carries out biochemical treatment；Feed liquid sampling detection, acetic acid content 81.9% in reactor.Instead
Answer kettle interlayer ON cycle water to cool, when temperature is down to 30 DEG C, phosphorus trichloride 8500kg is slowly added dropwise, temperature is kept during dropwise addition
Degree is no more than 40 DEG C, completion of dropwise addition, slowly heating esterification, when temperature rises to 110 DEG C, insulation reaction 2 hours, is slowly added to
2500kg deionized waters, are hydrolyzed；After hydrolysis terminates, distillation and acetic acid reception device are opened, heating distillation, receives acetic acid；
After concentration terminates, start punching and steam, 125 DEG C of temperature control is following, rushes after steaming terminates, addition 5000kg water, stirs；It is cooled to 95
DEG C, add hydrogen peroxide for decoloration, discharging.After testing, the active quantities that product is counted using acid continue to add water, adjust content as 67.15%
To 60%, other indexs meet industrial products requirement.
Embodiment 6
A kind of production technology that hydroxy ethylene diphosphonic acid is prepared using chloroacetic chloride waste liquid, using mass fraction as 70% chloroacetic chloride
Waste liquid, deionized water and phosphorus trichloride are raw material, according to step in detail below, complete production technology；Comprise the following steps that：Thoroughly
Clean the relevant devices, check valve, pressure etc. such as reactor, condenser；By 8000kg chloroacetic chloride waste liquids（GC detects butanone
3.9185%, chloroacetic chloride 66.2157%, acetic acid 22.3680%, aceticanhydride 3.4378%, reactor bottom is pumped into, opens stirring, condenser；
2000kg deionized waters are slowly added dropwise, temperature control is no more than 40 DEG C；After being added dropwise, 120 DEG C, in temperature-rise period are continuously heating to,
Front-end volatiles 1450kg is collected, sewage plant is delivered to and carries out biochemical treatment；Feed liquid sampling detection, acetic acid content 85.4% in reactor.Instead
Answer kettle interlayer ON cycle water to cool, when temperature is down to 30 DEG C, phosphorus trichloride 6900kg is slowly added dropwise, temperature is kept during dropwise addition
Degree is no more than 50 DEG C, completion of dropwise addition, slowly heating esterification, when temperature rises to 110 DEG C, insulation reaction 2 hours, is slowly added to
2000kg deionized waters, are hydrolyzed；After hydrolysis terminates, distillation and acetic acid reception device are opened, heating distillation, receives acetic acid；
After concentration terminates, start punching and steam, 125 DEG C of temperature control is following, rushes after steaming terminates, addition 4000kg water, stirs；It is cooled to 95
DEG C, add hydrogen peroxide for decoloration, discharging.After testing, for the active quantities that product is counted using acid as 60.88%, other indexs meet industry
Product requirement.
Active components of the HEDP produced by the invention in terms of HEDP is more than 98%；The isolated sterling acetic acid of this technique
Solution percentage composition is 70%-90%；The present invention has developed the technique that HEDP is prepared using chloroacetic chloride waste liquid, with traditional handicraft phase
Than improving the utilization ratio of chloroacetic chloride, realization is turned waste into wealth, and significantly reduces production cost.By the present invention, realize and contain
Impurity chloroacetic chloride is recycled, and the purity of byproduct acetic acid is higher, economizes on resources, and greatly reduces polyisobutylene phosphoric acid
The yield of " three wastes " in salt production process, the HEDP product indexs of preparation meet industrial products index.
Above-described embodiment is presently preferred embodiments of the present invention, is not the limitation to technical solution of the present invention, as long as
The technical scheme that can be realized on the basis of above-described embodiment without creative work, it is regarded as falling into patent of the present invention
Rights protection scope in.
Claims (2)
- A kind of 1. production technology that hydroxy ethylene diphosphonic acid is prepared using chloroacetic chloride waste liquid, it is characterised in that：With mass fraction It is raw material for 50-70% chloroacetic chloride waste liquid, deionized water and phosphorus trichloride, according to step in detail below, completes production technology； It is described to comprise the following steps that：（1）Thoroughly cleaning reactor, check valve, pressure；（2）1000 parts by weight chloroacetic chloride waste liquids are pumped into reactor bottom, open stirring；（3）Deionized water 150-450 parts by weight are slowly added dropwise, 10-50 DEG C of temperature control during dropwise addition, after completion of dropwise addition, stirring 2 is small When；Reaction equation：；（4）60-100 DEG C is continuously heating to, collects front-end volatiles 120-300 parts by weight, sewage plant is delivered to and carries out biochemical treatment；（5）Distillation terminates, and obtains acetum, and feed liquid sample examination in reactor, the acetic acid content is 70-90%；（6）ON cycle water, when material in reactor temperature is down to 30 DEG C, the parts by weight of phosphorus trichloride 1060 are slowly added dropwise, are added dropwise Process temperature control is at 10-50 DEG C；（7）After completion of dropwise addition, slowly heating esterification, when temperature rises to 105 DEG C, 1-4 hours are incubated；Reaction equation：；（8）The hydrolysis of 300 parts by weight of deionized water, hydrolysis time 2 hours is slowly added dropwise；（9）Distillation and dense time liquid reception device are opened, concentration distillation, receives acetum；（10）Rush steaming to terminate, add 250-400 parts by weight of deionized water, stir；（11）95 DEG C are cooled to, adds hydrogen peroxide for decoloration, is discharged, is examined.
- 2. a kind of production technology that hydroxy ethylene diphosphonic acid is prepared using chloroacetic chloride waste liquid according to claim 1, its It is characterised by：The step（2）In chloroacetic chloride waste liquid be containing acetic acid, butanone, aceticanhydride impurity chloroacetic chloride, the chloroacetic chloride accounts for The 50-70% of waste liquid gross mass, the acetic acid account for the 20-30% of waste liquid gross mass, and the butanone accounts for the 2-6% of waste liquid gross mass, institute State the 2-12% that aceticanhydride accounts for waste liquid gross mass.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1948258A (en) * | 2006-10-28 | 2007-04-18 | 周烜 | Preparation method and device of acetyl chloride and hydroxy ethylene diphosphonic acid coproduction |
| CN103319527A (en) * | 2013-07-08 | 2013-09-25 | 杨涛 | Production process for 1-hydroxy ethylidene-1,1-diphosphonic acid and acetylchloride |
| CN105622667A (en) * | 2015-12-31 | 2016-06-01 | 天津科维津宏环保科技有限公司 | Production method and system for co-production of acetyl chloride by 1-hydroxyethylidene-1,1-diphosphonicacid |
| CN106366124A (en) * | 2016-08-31 | 2017-02-01 | 南通联膦化工有限公司 | Production technology for preparing 1-hydroxyethylidene-1,1-diphosphonic acid from acetyl chloride waste liquid |
-
2017
- 2017-09-11 CN CN201710809614.8A patent/CN107602611A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1948258A (en) * | 2006-10-28 | 2007-04-18 | 周烜 | Preparation method and device of acetyl chloride and hydroxy ethylene diphosphonic acid coproduction |
| CN103319527A (en) * | 2013-07-08 | 2013-09-25 | 杨涛 | Production process for 1-hydroxy ethylidene-1,1-diphosphonic acid and acetylchloride |
| CN105622667A (en) * | 2015-12-31 | 2016-06-01 | 天津科维津宏环保科技有限公司 | Production method and system for co-production of acetyl chloride by 1-hydroxyethylidene-1,1-diphosphonicacid |
| CN106366124A (en) * | 2016-08-31 | 2017-02-01 | 南通联膦化工有限公司 | Production technology for preparing 1-hydroxyethylidene-1,1-diphosphonic acid from acetyl chloride waste liquid |
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Application publication date: 20180119 |