CN109534302A - A kind of method and its application for removing dimethyl sulfate in sulfuric acid - Google Patents
A kind of method and its application for removing dimethyl sulfate in sulfuric acid Download PDFInfo
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- CN109534302A CN109534302A CN201811348406.3A CN201811348406A CN109534302A CN 109534302 A CN109534302 A CN 109534302A CN 201811348406 A CN201811348406 A CN 201811348406A CN 109534302 A CN109534302 A CN 109534302A
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- sulfuric acid
- hydrogen peroxide
- dimethyl sulfate
- color
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/90—Separation; Purification
- C01B17/905—Removal of organic impurities
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Abstract
The method of dimethyl sulfate and its application in removal methane chloride sulfuric acid color in sulfuric acid are gone the invention discloses a kind of.The colour removal method includes the following steps: hydrogen peroxide to be added in the sulfuric acid of two formicester of sulfur acid, is sufficiently mixed, and reduction reaction generates methanol and sulfuric acid.Sulfuric acid colour removal method of the invention passes through nigrescence substance dimethyl sulfate redox reaction in oxidant hydrogen peroxide and sulfuric acid, dimethyl sulfate is reduced into sulfuric acid and methanol, to realize the Color removal of sulfuric acid product, the coloring matter in acid can be decomposed completely, obtains satisfactory recycling sulfuric acid, treatment process simple possible, it is easy to operate, it can be applied to the removal of methane chloride sulfuric acid color, the quality of dilute sulfuric acid can be promoted, be conducive to downstream client use, it is significant to environmental protection.
Description
Technical field
The present invention relates to chemical technology field, more particularly, to it is a kind of go in sulfuric acid the method for dimethyl sulfate and
It is applied
Background technique
Sulfuric acid is a kind of important industrial chemicals, can be used for manufacturing fertilizer, drug, explosive, pigment, detergent, battery
Deng being also widely used in purifying in the industry such as petroleum, metal smelt and dyestuff.With the rapid development of these industry, sulfuric acid
Consumption figure increases year by year, so that the discharge amount of sulfuric acid also increases with it, the retrieval of sulfuric acid containing color is utilized, and is not only advantageous to environment
Protection, the reasonable utilization to resource are also of great significance and act on.In methane chloride production process, sulfuric acid is used
In dry intermediate products monochloro methane, production when hydrogenation process methanol and chlorination hydrogenation should prepare monochloro methane in drying process
Raw by-product dimethyl ether and sulfuric acid reaction generates dimethyl sulfate, so as to cause sulfuric acid face used in methane chloride production
Color blacks, and can not normally recycle.At present removal methane chloride sulfuric acid color method have: thickening-purification technology method, air- extraction,
Freezing, extraction, absorption method, oxidizing process, thermal decomposition method, completely burned method, electrolysis method, dialysis, centrifugal process etc., but these
That there are processes is longer for method, and technics comparing is complicated, and processing cost is higher, and the energy consumption of consumption is high, not environmentally the disadvantages of.
Dimethyl suflfate category hypertoxic type, effect is similar to mustard gas, and acute toxicity is 15 times bigger than chlorine similar to phosgene.It is right
Eye, the upper respiratory tract have intense stimulus effect, have deep-etching effect to skin.Conjunctival congestion, oedema, corneal epithelium can be caused de-
It falls, trachea-bronchial epithelial cell epithelial cell partial necrosis, wearing out leads to vertical diaphragm or pneumoderm.Therefore it provides it is a kind of easy to operate and
The minimizing technology of the methane chloride dimethyl sulfate of environment-friendly high-efficiency just has very important meaning for the reuse of the sulfuric acid containing color
Justice.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the defects and deficiency of the existing reuse of sulfuric acid containing color, provide one kind and go
Except the method for methane chloride sulfuric acid color, removal is reacted with substance that show color dimethyl sulfate in sulfuric acid by oxidant hydrogen peroxide
Color, method are simple and efficient, and can completely remove methane chloride dilute sulfuric acid color.
Above-mentioned purpose of the present invention is achieved through the following technical solutions:
A method of dimethyl sulfate in sulfuric acid is removed, includes the following steps: the hydrogen peroxide two formicester of sulfur acid is added
Sulfuric acid in, be sufficiently mixed, reduction reaction generates methanol and sulfuric acid.
Dimethyl sulfate is yellow or black, recycles the face that can make sulfuric acid product in sulfuric acid product containing dimethyl sulfate
Color and quality are declined, the present invention provides it is a kind of removal recycling sulfuric acid product in dimethyl sulfate method, by
Oxidant hydrogen peroxide is added in recycling sulfuric acid, dimethyl sulfate is reduced into sulfuric acid and methanol, to realize the face of sulfuric acid product
Color removing, can decompose the coloring matter in acid completely, obtain satisfactory recycling sulfuric acid, specific reaction mechanism are as follows: (CH3)
2SO4+H2O2=H2SO4+2CH3OH.Present treatment simple process is feasible, easy to operate, using this method, can promote the product of dilute sulfuric acid
Matter is conducive to downstream client use, significant to environmental protection.
Preferably, the concentration of the hydrogen peroxide is 0.1~100%.
Preferably, the concentration of the hydrogen peroxide is 0.15~28.5%.
Preferably, the sulfuric acid adverse current of two formicester of the hydrogen peroxide and sulfur acid mixes, two formicester of hydrogen peroxide and sulfur acid
The flow-rate ratio of sulfuric acid is 1:6~20.
It can be decomposed completely by the ratio of control hydrogen peroxide and the sulfuric acid of two formicester of sulfur acid by being sufficiently mixed stirring
Coloring matter in acid.Adverse current mixing can be poor using the concentration gradient of the two, and is conducive to increase the time of contact of reaction and connect
Contacting surface product makes, and must react more abundant
Preferably, the dosage of the hydrogen peroxide is 0.5~100 times of dimethyl sulfate quality in sulfuric acid.
Preferably, the dosage of the hydrogen peroxide is 1~10 times of dimethyl sulfate quality in sulfuric acid.
Preferably, 50.0~166.6kg of hydrogen peroxide is added in the sulfuric acid of two formicester of sulfur acid per ton.
A kind of application of the above method in removal methane chloride sulfuric acid color.Methane chloride sulfuric acid is black
Main cause are as follows: in methane chloride production process, when hydrogenation process methanol and chlorination hydrogenation should prepare monochloro methane, produce
Raw by-product dimethyl ether and sulfuric acid reaction generates dimethyl sulfate, so that the sulfuric acid color in monochloro methane drying tower is sent out
It is black, influence subsequent recovery utilization, specific reaction mechanism are as follows:
2CH3OH=H3COCH3+H2O
CH3OCH3+SO3=(CH3)2SO4
(CH3)2SO4+H2O2=H2SO4+2CH3OH
The nigrescence substance sulfuric acid in sulfuric acid can be effectively removed using the method for removing dimethyl sulfate in sulfuric acid of the invention
Two formicesters, to effectively remove sulfuric acid color, hydrogen peroxide can also remove the free chlorine in sulfuric acid, and the sulfuric acid after removing color can
It is for sale.
Preferably, isolated qualified dilute sulfuric acid is sprayed after restoring the sulfuric acid removing particulate matter of generation.After being restored after reaction
Dilute sulfuric acid, the sulfuric acid containing particle sprays from qualified acid tank groove top and separates after filtering, and methane removes tail gas absorbing system, closes
Lattice dilute sulfuric acid drops down onto slot.
Preferably, the particulate matter is removed by secondary filter.Other granular solids objects in sulfuric acid that drying tower comes out
Matter is intercepted by accurate filter.
Compared with prior art, the beneficial effects of the present invention are:
The present invention provides a kind of methods for removing dimethyl sulfate in sulfuric acid, by sending out in oxidant hydrogen peroxide and sulfuric acid
Black substance dimethyl sulfate redox reaction, is reduced into sulfuric acid and methanol for dimethyl sulfate, to realize sulfuric acid product
Color removal can decompose the coloring matter in acid completely, obtain satisfactory recycling sulfuric acid, treatment process simple possible, behaviour
Facilitate, can be applied to the removal of methane chloride sulfuric acid color, the quality of dilute sulfuric acid can be promoted, being conducive to downstream client makes
With to environmentally friendly significant.
Specific embodiment
The present invention is further illustrated With reference to embodiment, but embodiment the present invention is not done it is any
The restriction of form.Unless otherwise indicated, source chemicals used in the embodiment of the present invention are the source chemicals routinely bought.
Embodiment 1
A method of removal methane chloride sulfuric acid color, comprising the following steps:
(1) by the sulfuric acid of methane chloride (76%) 20m3/ h, the hydrogen peroxide solution 1m with 27.5%3/ h mixing, hydrogen peroxide
It is chemically reacted with dimethyl sulfate, is reduced into methanol and sulfuric acid.
(2) sulfuric acid in step (1) after reduction intercepts removal particulate matter by accurate filter, from qualified sulfuric acid tank slot
Top spray leaching separation, tail gas remove tail gas absorbing system, and qualified sulfuric acid drops down onto slot.
Treatment effect is shown in Table 1.
1. sulfuric acid of table (76%) contrast table before and after the processing
| Color | Concentration (%) | Temperature DEG C | Dimethyl sulfate content/% | |
| Dilute sulfuric acid before handling | Black | 76.0 | 30 | 6.4 |
| Dilute sulfuric acid after processing | It is colourless | 76.0 | 31 | 1.2 |
Embodiment 2
A method of removal methane chloride sulfuric acid color, comprising the following steps:
(1) by the sulfuric acid of methane chloride (76%) 20m3/ h, the hydrogen peroxide solution 1.5m with 27.5%3/ h mixing, dioxygen
Water is chemically reacted with dimethyl sulfate, is reduced into methanol and sulfuric acid.
(2) sulfuric acid in step (1) after reduction intercepts removal particulate matter by accurate filter, from qualified dilute sulfuric acid tank
Groove top spray separation, tail gas remove tail gas absorbing system, and qualified sulfuric acid drops down onto slot.
Treatment effect is shown in Table 2.
2. sulfuric acid of table (76%) contrast table before and after the processing
Embodiment 3
A method of removal methane chloride sulfuric acid color, comprising the following steps:
(1) by the sulfuric acid of methane chloride (76%) 20m3/ h, the hydrogen peroxide solution 1.5m with 28.5%3/ h mixing, dioxygen
Water is chemically reacted with dimethyl sulfate, is reduced into methanol and sulfuric acid.
(2) sulfuric acid in step (1) after reduction intercepts removal particulate matter by accurate filter, from qualified dilute sulfuric acid tank
Groove top spray separation, tail gas remove tail gas absorbing system, and qualified sulfuric acid drops down onto slot.
Processing result is shown in 3.
3. sulfuric acid of table (76%) contrast table before and after the processing
| Color | Concentration (%) | Temperature DEG C | Dimethyl sulfate content/% | |
| Dilute sulfuric acid before handling | Black | 76.0 | 30 | 6.4 |
| Dilute sulfuric acid after processing | It is colourless | 76.0 | 31 | 0 |
Embodiment 4
A method of removal methane chloride sulfuric acid color, comprising the following steps:
(1) by the sulfuric acid of methane chloride (76%) 20m3/ h, the hydrogen peroxide solution 1.5m with 0.5%3/ h mixing, dioxygen
Water is chemically reacted with dimethyl sulfate, is reduced into methanol and sulfuric acid.
(2) sulfuric acid in step (1) after reduction intercepts removal particulate matter by accurate filter, from qualified dilute sulfuric acid tank
Groove top spray separation, tail gas remove tail gas absorbing system, and qualified sulfuric acid drops down onto slot.
Processing result is shown in 4.
4. sulfuric acid of table (76%) contrast table before and after the processing
| Color | Concentration (%) | Temperature DEG C | Dimethyl sulfate content/% | |
| Dilute sulfuric acid before handling | Black | 76.0 | 30 | 6.4 |
| Dilute sulfuric acid after processing | Brown | 76.0 | 31 | 2.9 |
Embodiment 5
A method of removal methane chloride sulfuric acid color, comprising the following steps:
(1) by the sulfuric acid of methane chloride (76%) 10m3/ h, the hydrogen peroxide solution 1.5m with 7%3/ h mixing, hydrogen peroxide
It is chemically reacted with dimethyl sulfate, is reduced into methanol and sulfuric acid.
(2) sulfuric acid in step (1) after reduction intercepts removal particulate matter by accurate filter, from qualified dilute sulfuric acid tank
Groove top spray separation, tail gas remove tail gas absorbing system, and qualified sulfuric acid drops down onto slot.
Processing result is shown in 5.
5. sulfuric acid of table (76%) contrast table before and after the processing
| Color | Concentration (%) | Temperature DEG C | Dimethyl sulfate content/% | |
| Dilute sulfuric acid before handling | Black | 76.0 | 30 | 6.4 |
| Dilute sulfuric acid after processing | Brown | 76.0 | 31 | 2.9 |
Embodiment 6
A method of removal methane chloride sulfuric acid color, comprising the following steps:
(1) by the sulfuric acid of methane chloride (76%) 6m3/ h, the hydrogen peroxide solution 1.5m with 7%3/ h mixing, hydrogen peroxide with
Dimethyl sulfate chemically reacts, and is reduced into methanol and sulfuric acid.
(2) sulfuric acid in step (1) after reduction intercepts removal particulate matter by accurate filter, from qualified dilute sulfuric acid tank
Groove top spray separation, tail gas remove tail gas absorbing system, and qualified sulfuric acid drops down onto slot.
Processing result is shown in 6.
6. sulfuric acid of table (76%) contrast table before and after the processing
| Color | Concentration (%) | Temperature DEG C | Dimethyl sulfate content/% | |
| Dilute sulfuric acid before handling | Black | 76.0 | 30 | 6.4 |
| Dilute sulfuric acid after processing | It is colourless | 76.0 | 31 | 0 |
Embodiment 7
A method of removal methane chloride sulfuric acid color, comprising the following steps:
(1) sulfuric acid of methane chloride (76%) is mixed with 0.15% hydrogen peroxide solution, hydrogen peroxide and dimethyl sulfate
Rouge chemically reacts, and is reduced into methanol and sulfuric acid, and the dosage of hydrogen peroxide is 0.5 times of dimethyl sulfate quality in sulfuric acid.
(2) sulfuric acid in step (1) after reduction intercepts removal particulate matter by accurate filter, from qualified dilute sulfuric acid tank
Groove top spray separation, tail gas remove tail gas absorbing system, and qualified sulfuric acid drops down onto slot.
Processing result is shown in 7.
7. sulfuric acid of table (76%) contrast table before and after the processing
| Color | Concentration (%) | Temperature DEG C | Dimethyl sulfate content/% | |
| Dilute sulfuric acid before handling | Black | 76.0 | 30 | 6.4 |
| Dilute sulfuric acid after processing | Brown | 76.0 | 31 | 3.1 |
Embodiment 8
A method of removal methane chloride sulfuric acid color, comprising the following steps:
(1) sulfuric acid of methane chloride (76%) is mixed with 0.15% hydrogen peroxide solution, hydrogen peroxide and dimethyl sulfate
Rouge chemically reacts, and is reduced into methanol and sulfuric acid, and the dosage of hydrogen peroxide is 10 times of dimethyl sulfate quality in sulfuric acid.
(2) sulfuric acid in step (1) after reduction intercepts removal particulate matter by accurate filter, from qualified dilute sulfuric acid tank
Groove top spray separation, tail gas remove tail gas absorbing system, and qualified sulfuric acid drops down onto slot.
Processing result is shown in 8.
8. sulfuric acid of table (76%) contrast table before and after the processing
| Color | Concentration (%) | Temperature DEG C | Dimethyl sulfate content/% | |
| Dilute sulfuric acid before handling | Black | 76.0 | 30 | 6.4 |
| Dilute sulfuric acid after processing | It is colourless | 76.0 | 31 | 0.75 |
Embodiment 9
A method of removal methane chloride sulfuric acid color, comprising the following steps:
(1) sulfuric acid of methane chloride (76%) is mixed with 0.15% hydrogen peroxide solution, hydrogen peroxide and dimethyl sulfate
Rouge chemically reacts, and is reduced into methanol and sulfuric acid, and the dosage of hydrogen peroxide is 100 times of dimethyl sulfate quality in sulfuric acid.
(2) sulfuric acid in step (1) after reduction intercepts removal particulate matter by accurate filter, from qualified dilute sulfuric acid tank
Groove top spray separation, tail gas remove tail gas absorbing system, and qualified sulfuric acid drops down onto slot.
Processing result is shown in 9.
9. sulfuric acid of table (76%) contrast table before and after the processing
| Color | Concentration (%) | Temperature DEG C | Dimethyl sulfate content/% | |
| Dilute sulfuric acid before handling | Black | 76.0 | 30 | 6.4 |
| Dilute sulfuric acid after processing | It is colourless | 76.0 | 31 | 0 |
Embodiment 10
A method of removal methane chloride sulfuric acid color, comprising the following steps:
(1) sulfuric acid of methane chloride (76%) is mixed with 0.15% hydrogen peroxide solution, hydrogen peroxide and dimethyl sulfate
Rouge chemically reacts, and is reduced into methanol and sulfuric acid, and the dosage of hydrogen peroxide is 1 times of dimethyl sulfate quality in sulfuric acid.
(2) sulfuric acid in step (1) after reduction intercepts removal particulate matter by accurate filter, from qualified dilute sulfuric acid tank
Groove top spray separation, tail gas remove tail gas absorbing system, and qualified sulfuric acid drops down onto slot.
Processing result is shown in 10.
10. sulfuric acid of table (76%) contrast table before and after the processing
| Color | Concentration (%) | Temperature DEG C | Dimethyl sulfate content/% | |
| Dilute sulfuric acid before handling | Black | 76.0 | 30 | 6.4 |
| Dilute sulfuric acid after processing | Brown | 76.0 | 31 | 2.8 |
Embodiment 11
A method of removal methane chloride sulfuric acid color, comprising the following steps:
(1) sulfuric acid of methane chloride (76%) is mixed with 27.5% hydrogen peroxide solution, hydrogen peroxide and dimethyl sulfate
Rouge chemically reacts, and is reduced into methanol and sulfuric acid, hydrogen peroxide 50.00kg is added in the sulfuric acid of two formicester of sulfur acid per ton.
(2) sulfuric acid in step (1) after reduction intercepts removal particulate matter by accurate filter, from qualified dilute sulfuric acid tank
Groove top spray separation, tail gas remove tail gas absorbing system, and qualified sulfuric acid drops down onto slot.
Processing result is shown in 11.
11. sulfuric acid of table (76%) contrast table before and after the processing
| Color | Concentration (%) | Temperature DEG C | Dimethyl sulfate content/% | |
| Dilute sulfuric acid before handling | Black | 76.0 | 30 | 6.4 |
| Dilute sulfuric acid after processing | It is colourless | 76.0 | 31 | 1.2 |
Embodiment 12
A method of removal methane chloride sulfuric acid color, comprising the following steps:
(1) sulfuric acid of methane chloride (76%) is mixed with 27.5% hydrogen peroxide solution, hydrogen peroxide and dimethyl sulfate
Rouge chemically reacts, and is reduced into methanol and sulfuric acid, hydrogen peroxide 166.00kg is added in the sulfuric acid of two formicester of sulfur acid per ton.
(2) sulfuric acid in step (1) after reduction intercepts removal particulate matter by accurate filter, from qualified dilute sulfuric acid tank
Groove top spray separation, tail gas remove tail gas absorbing system, and qualified sulfuric acid drops down onto slot.
Processing result is shown in 12.
12. sulfuric acid of table (76%) contrast table before and after the processing
| Color | Concentration (%) | Temperature DEG C | Dimethyl sulfate content/% | |
| Dilute sulfuric acid before handling | Black | 76.0 | 30 | 6.4 |
| Dilute sulfuric acid after processing | It is colourless | 76.0 | 31 | 0 |
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention.For those of ordinary skill in the art, may be used also on the basis of the above description
To make other variations or changes in different ways.There is no necessity and possibility to exhaust all the enbodiments.It is all this
Made any modifications, equivalent replacements, and improvements etc., should be included in the claims in the present invention within the spirit and principle of invention
Protection scope within.
Claims (10)
1. a kind of method for removing dimethyl sulfate in sulfuric acid, which comprises the steps of: sulfur-bearing is added in hydrogen peroxide
It in the sulfuric acid of sour two formicesters, is sufficiently mixed, reduction reaction generates methanol and sulfuric acid.
2. method as described in claim 1, which is characterized in that the concentration of the hydrogen peroxide is 0.1 ~ 100%.
3. method as claimed in claim 2, which is characterized in that the concentration of the hydrogen peroxide is 0.15 ~ 28.5%.
4. method as described in claim 1, which is characterized in that the sulfuric acid adverse current of two formicester of the hydrogen peroxide and sulfur acid mixes,
The flow-rate ratio of the sulfuric acid of two formicester of hydrogen peroxide and sulfur acid is 1:6 ~ 20.
5. method as described in claim 1, which is characterized in that the dosage of the hydrogen peroxide is dimethyl sulfate quality in sulfuric acid
0.5 ~ 100 times.
6. method as claimed in claim 5, which is characterized in that the dosage of the hydrogen peroxide is dimethyl sulfate quality in sulfuric acid
1 ~ 10 times.
7. method as described in claim 1, which is characterized in that in the sulfuric acid of two formicester of sulfur acid per ton be added hydrogen peroxide 50.0 ~
166.6kg。
8. a kind of application of claim 1 ~ 7 any one the method in removal methane chloride sulfuric acid color.
9. application as claimed in claim 8, which is characterized in that spray isolated conjunction after restoring the sulfuric acid removing particulate matter of generation
Lattice dilute sulfuric acid.
10. method as claimed in claim 9, which is characterized in that the particulate matter is removed by secondary filter.
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| CN201811348406.3A CN109534302A (en) | 2018-11-13 | 2018-11-13 | A kind of method and its application for removing dimethyl sulfate in sulfuric acid |
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