CN107602610A - It is a kind of can reuse sulfuric acid wastewater containing organic phospho acid production technology - Google Patents
It is a kind of can reuse sulfuric acid wastewater containing organic phospho acid production technology Download PDFInfo
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- CN107602610A CN107602610A CN201710808353.8A CN201710808353A CN107602610A CN 107602610 A CN107602610 A CN 107602610A CN 201710808353 A CN201710808353 A CN 201710808353A CN 107602610 A CN107602610 A CN 107602610A
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Abstract
The invention discloses it is a kind of can reuse sulfuric acid wastewater containing organic phospho acid production technology, using sulfuric acid wastewater containing, phosphorous acid, hydrogen chloride gas, formaldehyde, organic amine as raw material, by following steps complete can reuse sulfuric acid wastewater containing organic phospho acid production technology；The invention provides it is a kind of can reuse sulfuric acid wastewater containing organic phospho acid production technology, sulfuric acid consumption significantly reduces, significantly reduce production cost, greatly reduce waste water generation, wastewater sources control is realized, the present invention is operated, had no irritating odor in confined conditions, reduce the yield of " three wastes ", it is environmentally friendly.
Description
Technical field
The present invention relates to a kind of production technology of organic phospho acid, and in particular to it is a kind of can reuse sulfuric acid wastewater containing organic phospho acid
Production technology.
Background technology
The agent of organic inhibition dirty-proof containing phosphine has turned into be most widely used and successful a kind of water stabilization in Treatment of Industrial Water
Agent.Their chemical stability is good, not facile hydrolysis, and high temperature resistant, will not be led in use because hydrolysis generates orthophosphates
Cause bacterium algae excessive multiplication.Organic phosphonate also has critical value effect as Quadrafos, exactly need to only use 3-5 milligrams per liter
Organic phospho acid prevents from 400mg/L precipitation of calcium carbonate；It is used in combination and can shows with other water treatment agents under certain condition
Go out preferable cooperative effect, have corrosion-mitigation scale-inhibition effect concurrently.Organic phospho acid also has good corrosion inhibition at high doses, and
Belong to nontoxic or less toxic medicament.It has been widely used in water treatment agent, metal conditioner, electronics industry cleaning agent, day
With fields such as chemical additives.
According to the preparation technology of existing organic phospho acid and its salt, typically using sulfuric acid, formaldehyde, organic amine as raw material, this
Kind preparation technology, sulfuric acid, formaldehyde consumption are all bigger, and the largely waste water containing sulfuric acid can be produced in production process, give up
Sulfuric acid content is 10% or so in water, while also contains 1-2% formaldehyde, low by biochemical treatment possibility, therefore development can reuse
The preparation technology of the organic phospho acid of sulfuric acid wastewater containing is the effective measures of blowdown of economizing on resources, reduce.
The content of the invention
A large amount of sulphur are produced in view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to now provide one kind and solve existing process
The drawbacks of sour waste water, improve sulfuric acid service efficiency, production cost be greatly reduced, greatly reduce caused by sewage can reuse sulfuric acid give up
The production technology of the organic phospho acid of water.
In order to solve the above technical problems, the technical solution adopted by the present invention is：It is a kind of can reuse sulfuric acid wastewater containing organic phosphine
The production technology of acid, its innovative point are：Using sulfuric acid wastewater containing, phosphorous acid, hydrogen chloride gas, formaldehyde, organic amine as raw material, pass through
Following steps complete can reuse sulfuric acid wastewater containing organic phospho acid production technology, it is described to comprise the following steps that：
（1）Sulfuric acid storage tank and relevant device are cleaned, storage tank valve is closed in place；
（2）1200 parts sulfuric acid waste water are pumped into sulfuric acid storage tank；
（3）Hydrogen chloride gas, ON cycle and falling film absorbing device are passed through into storage tank；
（4）Hydrogen chloride gas is passed through, sulfuric acid concentration is judged according to the B that storage tank is subsidiary；
（5）When Baume degrees, which reaches specified, to be required, stopping is passed through hydrogen chloride gas, samples, and chemically examines sulfuric acid waste content, will detect
Sulfuric acid after qualified is pumped into storage tank, standby；
（6）According to the production technology of different organic phosphines, step is put into proportion（5）It is the sulfuric acid of preparation, phosphorous acid, formaldehyde, organic
Amine raw material prepares organic phospho acid, and caused sulfuric acid wastewater containing in production process is reclaimed.
Further, the step（2）In, the mass fraction of sulfuric acid wastewater containing is 8-10%.
Further, the step（4）In, lead to the mass parts of hydrogen chloride gas in 380-420 parts.
Further, the step（5）In, for B reading between 20-22, sulfuric acid waste content is 32-40%.
Further, the step（6）In, organic amine be diglycolamine, ethylenediamine, polyetheramine, diethylenetriamine, oneself two
One kind in amine, double 1,6- hexamethylene triamines.
Beneficial effects of the present invention are as follows：The invention provides it is a kind of can reuse sulfuric acid wastewater containing organic phospho acid production work
Skill, sulfuric acid consumption significantly reduce, and significantly reduce production cost, greatly reduce waste water generation, realize wastewater sources control
System, the present invention operates, has no irritating odor, reduce the yield of " three wastes " in confined conditions, environmentally friendly.
Brief description of the drawings
Fig. 1 is the diethylene triamine pentamethylene phosphonic 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 diethylene triamine pentamethylene phosphonic process chart of the present invention, with the methene of diethylenetriamine five
Exemplified by phosphonic acids, it is specifically addressed.
It is a kind of can reuse sulfuric acid wastewater containing organic phospho acid production technology, using phosphorous acid, sulfuric acid, formaldehyde, organic amine as original
Material, by following steps complete can reuse sulfuric acid wastewater containing organic phospho acid production technology, comprise the following steps that：
（1）Sulfuric acid storage tank and relevant device are cleaned, storage tank valve is closed in place；
（2）1200 parts sulfuric acid waste water are pumped into sulfuric acid storage tank；
（3）Hydrogen chloride gas, ON cycle and falling film absorbing device are passed through into storage tank；
（4）Hydrogen chloride gas is passed through, sulfuric acid concentration is judged according to the B that storage tank is subsidiary；
（5）When Baume degrees, which reaches specified, to be required, stopping is passed through hydrogen chloride gas, samples, and chemically examines sulfuric acid waste content, will detect
Sulfuric acid after qualified is pumped into storage tank, standby；
（6）According to the production technology of different organic phosphines, step is put into proportion（5）It is the sulfuric acid of preparation, phosphorous acid, formaldehyde, organic
Amine raw material prepares organic phospho acid, and caused sulfuric acid wastewater containing in production process is reclaimed.
As embodiment, more specifically embodiment is step（2）In, the mass fraction of sulfuric acid wastewater containing is 8-10%, step
Suddenly（4）In, lead to the mass parts of hydrogen chloride gas in 380-420 parts, step（5）In, B reading is between 20-22, sulfuric acid
Waste liquid content is 32-40%, step（6）In, organic amine be diglycolamine, ethylenediamine, polyetheramine, diethylenetriamine, hexamethylene diamine,
One kind in double 1,6- hexamethylene triamines.
Embodiment 1
It is a kind of can reuse sulfuric acid wastewater containing organic phospho acid production technology, concretely comprise the following steps：Clean sulfuric acid storage tank and its relevant tube
Road, check valve, pressure；5000kg sulfuric acid wastewater containings are pumped into sulfuric acid storage tank, open each valve of air inducing pipeline, confirm falling film absorption
Balanced valve is opened between device and storage tank, is opened and is absorbed storage tank water-circulating pump valve, confirms that other valves are inhaled in correct position, unlatching tail gas
Receive pump and spray pump and check equipment normal operation, press circulating pump shift knob, start circulating pump circularly absorbing hydrogen chloride, together
Shi Kaiqi falling-film absorber cooling circulating waters, absorb 4 hours, tourie Baume measurement concentration is 20.5-21.5, stops absorbing chlorine
Change hydrogen, sample examination, hydrogen chloride content 35.3%.
Clean reactor and relevant device, check valve, pressure；2700kg phosphorous acid is pumped into reactor, then by sulphur
Sulfuric acid 1800kg prepared by sour waste water squeezes into reactor, opens stirring；Diethylenetriamine 540kg is slowly added dropwise；Steam is warming up to
75 DEG C, start that formalin, time for adding 2 hours is added dropwise.After being added dropwise, insulation reaction 2 hours, temperature is raised to 105 DEG C,
Back flow reaction 2 hours.Heating concentration, recovery sulfuric acid waste to sulfuric acid storage tank；100KG deionized waters are added into kettle twice, are added
Heat concentration, recovery sulfuric acid waste to sulfuric acid storage tank；2250KG deionized waters are added into reactor, are cooled down, filtering.After testing,
For product using the active quantities that organic phospho acid is counted as 50.12%, all indexs meet the methene phosphine of normal commercial level diethylenetriamine five
Acid.
Embodiment 2
It is a kind of can reuse sulfuric acid wastewater containing organic phospho acid production technology, concretely comprise the following steps：Clean sulfuric acid storage tank and its relevant tube
Road, check valve, pressure；5000kg sulfuric acid wastewater containings are pumped into sulfuric acid storage tank, open each valve of air inducing pipeline, confirm falling film absorption
Balanced valve is opened between device and storage tank, is opened and is absorbed storage tank water-circulating pump valve, confirms other valves in correct position.Tail gas is opened to inhale
Receive pump and spray pump and check equipment normal operation, press circulating pump shift knob, start circulating pump circularly absorbing hydrogen chloride, together
Shi Kaiqi falling-film absorber cooling circulating waters, absorb 3 hours, tourie Baume measurement concentration is 20-21, stops absorbing chlorination
Hydrogen.Sample examination, hydrogen chloride content 34.3%.
Clean reactor and relevant device, check valve, pressure；2700kg phosphorous acid is pumped into reactor, then by sulphur
Sulfuric acid 1880kg prepared by sour waste water squeezes into reactor, opens stirring；Diethylenetriamine 540kg is slowly added dropwise；Steam is warming up to
75 DEG C, start that formalin is added dropwise, time for adding 2 hours, after being added dropwise, insulation reaction 2 hours, raise temperature to 105 DEG C,
Back flow reaction 2 hours, heating concentration, recovery sulfuric acid waste to sulfuric acid storage tank；100KG deionized waters are added into kettle twice, are added
Heat concentration, recovery sulfuric acid waste to sulfuric acid storage tank；2250KG deionized waters are added into reactor, are cooled down, filtering, after testing,
For product using the active quantities that organic phospho acid is counted as 49.18%, all indexs meet the methene phosphine of normal commercial level diethylenetriamine five
Acid.
Embodiment 3
It is a kind of can reuse sulfuric acid wastewater containing organic phospho acid production technology, concretely comprise the following steps：Clean sulfuric acid storage tank and its relevant tube
Road, check valve, pressure；5000kg sulfuric acid wastewater containings are pumped into sulfuric acid storage tank, open each valve of air inducing pipeline, confirm falling film absorption
Balanced valve is opened between device and storage tank, is opened and is absorbed storage tank water-circulating pump valve, confirms that other valves are inhaled in correct position, unlatching tail gas
Receive pump and spray pump and check equipment normal operation, press circulating pump shift knob, start circulating pump circularly absorbing hydrogen chloride, together
Shi Kaiqi falling-film absorber cooling circulating waters, absorb 5 hours, tourie Baume measurement concentration is 21-22, stops absorbing chlorination
Hydrogen, sample examination, hydrogen chloride content 36.2%.
Clean reactor and relevant device, check valve, pressure；2700kg phosphorous acid is pumped into reactor, then by sulphur
Sulfuric acid 1780kg prepared by sour waste water squeezes into reactor, opens stirring；Diethylenetriamine 540kg is slowly added dropwise；Steam is warming up to
75 DEG C, start that formalin is added dropwise, time for adding 2 hours, after being added dropwise, insulation reaction 2 hours, raise temperature to 105 DEG C,
Back flow reaction 2 hours, heating concentration, recovery sulfuric acid waste to sulfuric acid storage tank；100KG deionized waters are added into kettle twice, are added
Heat concentration, recovery sulfuric acid waste to sulfuric acid storage tank；2250KG deionized waters are added into reactor, are cooled down, filtering, after testing,
For product using the active quantities that organic phospho acid is counted as 50.97%, all indexs meet the methene phosphine of normal commercial level diethylenetriamine five
Acid.
The invention provides it is a kind of can reuse sulfuric acid wastewater containing organic phospho acid production technology, sulfuric acid consumption substantially subtracts
It is few, production cost is significantly reduced, greatly reduces waste water generation, realizes wastewater sources control, the present invention is in airtight condition
Lower operation, has no irritating odor, and reduces the yield of " three wastes ", environmentally friendly.
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 (5)
1. it is a kind of can reuse sulfuric acid wastewater containing organic phospho acid production technology, it is characterised in that：With sulfuric acid wastewater containing, phosphorous acid, chlorine
Change hydrogen, formaldehyde, organic amine be raw material, by following steps completion can reuse sulfuric acid wastewater containing organic phospho acid production work
Skill, it is described to comprise the following steps that：
（1）Sulfuric acid storage tank and relevant device are cleaned, storage tank valve is closed in place；
（2）1200 parts sulfuric acid waste water are pumped into sulfuric acid storage tank；
（3）Hydrogen chloride gas, ON cycle and falling film absorbing device are passed through into storage tank；
（4）Hydrogen chloride gas is passed through, sulfuric acid concentration is judged according to the B that storage tank is subsidiary；
（5）When Baume degrees, which reaches specified, to be required, stopping is passed through hydrogen chloride gas, samples, and chemically examines sulfuric acid waste content, will detect
Sulfuric acid after qualified is pumped into storage tank, standby；
（6）According to the production technology of different organic phosphines, step is put into proportion（5）It is the sulfuric acid of preparation, phosphorous acid, formaldehyde, organic
Amine raw material prepares organic phospho acid, and caused sulfuric acid wastewater containing in production process is reclaimed.
2. it is according to claim 1 it is a kind of can reuse sulfuric acid wastewater containing organic phospho acid production technology, it is characterised in that：Institute
State step（2）In, the mass fraction of sulfuric acid wastewater containing is 8-10%.
3. it is according to claim 1 it is a kind of can reuse sulfuric acid wastewater containing organic phospho acid production technology, it is characterised in that：Institute
State step（4）In, lead to the mass parts of hydrogen chloride gas in 380-420 parts.
4. it is according to claim 1 it is a kind of can reuse sulfuric acid wastewater containing organic phospho acid production technology, it is characterised in that：Institute
State step（5）In, for B reading between 20-22, sulfuric acid waste content is 32-40%.
5. it is according to claim 1 it is a kind of can reuse sulfuric acid wastewater containing organic phospho acid production technology, it is characterised in that：Institute
State step（6）In, organic amine is diglycolamine, ethylenediamine, polyetheramine, diethylenetriamine, hexamethylene diamine, double 1,6- hexamethylene triamines
In one kind.
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| CN201710808353.8A CN107602610A (en) | 2017-09-09 | 2017-09-09 | It is a kind of can reuse sulfuric acid wastewater containing organic phospho acid production technology |
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| CN201710808353.8A CN107602610A (en) | 2017-09-09 | 2017-09-09 | It is a kind of can reuse sulfuric acid wastewater containing organic phospho acid production technology |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110804071A (en) * | 2019-11-08 | 2020-02-18 | 山东泰和水处理科技股份有限公司 | Production method of diethylenetriamine pentamethylene phosphonic acid |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1218477A (en) * | 1996-04-12 | 1999-06-02 | 洛夫斯格罗夫研究有限公司 | Organo phosphorous compounds |
| CN106366123A (en) * | 2016-08-31 | 2017-02-01 | 南通联膦化工有限公司 | Production process of organic phosphonic acid of recyclable hydrochloric acid wastewater |
| CN106518919A (en) * | 2016-08-31 | 2017-03-22 | 南通联膦化工有限公司 | Technology used for producing amino trimethylene phosphoric acid and salts thereof and capable of reusing formaldehyde wastewater |
-
2017
- 2017-09-09 CN CN201710808353.8A patent/CN107602610A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1218477A (en) * | 1996-04-12 | 1999-06-02 | 洛夫斯格罗夫研究有限公司 | Organo phosphorous compounds |
| CN106366123A (en) * | 2016-08-31 | 2017-02-01 | 南通联膦化工有限公司 | Production process of organic phosphonic acid of recyclable hydrochloric acid wastewater |
| CN106518919A (en) * | 2016-08-31 | 2017-03-22 | 南通联膦化工有限公司 | Technology used for producing amino trimethylene phosphoric acid and salts thereof and capable of reusing formaldehyde wastewater |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110804071A (en) * | 2019-11-08 | 2020-02-18 | 山东泰和水处理科技股份有限公司 | Production method of diethylenetriamine pentamethylene phosphonic acid |
| CN110804071B (en) * | 2019-11-08 | 2021-09-17 | 山东泰和水处理科技股份有限公司 | Production method of diethylenetriamine pentamethylene phosphonic acid |
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