CN111792623A - Method for recovering and preparing high-quality hydrochloric acid from waste gas of phosgene reaction system - Google Patents
Method for recovering and preparing high-quality hydrochloric acid from waste gas of phosgene reaction system Download PDFInfo
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- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
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- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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Abstract
The invention discloses a method for recovering and preparing high-quality hydrochloric acid from waste gas of a phosgene reaction system, which comprises the following steps: absorbing the waste gas in a phosgene reaction system by using water to obtain recovered hydrochloric acid; and adsorbing the recovered hydrochloric acid by adopting macroporous resin and activated carbon to obtain high-quality hydrochloric acid. According to the invention, water is firstly adopted to adsorb the waste gas in the phosgene reaction system, so that hydrogen chloride is dissolved in the water, the recovered hydrochloric acid is further adsorbed by macroporous resin and activated carbon, the pungent phosgene smell in the recovered hydrochloric acid or the purified hydrochloric acid is removed, and impurities (colors) in the purified hydrochloric acid are removed, so that the recovered hydrochloric acid becomes colorless and transparent, and the high-quality hydrochloric acid is obtained.
Description
Technical Field
The invention relates to a recovery process for purifying hydrogen chloride gas by a physical separation method, in particular to a method for recovering and preparing high-quality hydrochloric acid from waste gas of a phosgene reaction system.
Background
The phosgene reaction system refers to a reaction involving phosgene as a raw material, for example, methyl isocyanate is produced by producing phosgene and methylamine, o-hydroxybenzonitrile is produced by reacting phosgene and salicylamide, many acyl chloride products are synthesized by reacting phosgene and corresponding organic acid, and the phosgene reaction generates a large amount of reaction waste gas, and the main components of the waste gas are carbon monoxide, phosgene and hydrogen chloride.
At present, the method for recovering and treating the waste gas of a phosgene reaction system mainly comprises the steps of directly spraying the waste gas of the phosgene reaction system by using water, absorbing the waste gas of the phosgene reaction system by using the water to obtain a recovered hydrochloric acid solution, and because the recovered hydrochloric acid solution generally has dark yellow to red color and has strong phosgene smell, the method can only be used for ore washing and rust removal, and has low economic benefit. However, under the influence of the national environmental protection policy, the ore washing industry is gradually declined, the demand of hydrochloric acid is also reduced year by year, and if the byproduct hydrochloric acid cannot be timely treated, the byproduct hydrochloric acid can only be stored in a plurality of large tanks of a factory, so that the whole production operation is influenced, and even the production is stopped due to the expansion of the hydrochloric acid. In addition, reports on recovery and preparation of high-quality hydrochloric acid from the exhaust gas of a phosgene reaction system have not been found in the prior art. In addition, the existing waste hydrochloric acid recovery process mainly adopts steam and calcium chloride to recover and purify hydrochloric acid, but the steam used in the methods has higher energy consumption and relates to the later recovery of the calcium chloride, and compared with the selling price of the hydrochloric acid, the treatment cost is relatively higher, so that the recovery processes have no practical application value.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects of the prior art and provide the method for recovering and preparing the high-quality hydrochloric acid from the waste gas of the phosgene reaction system, which has the advantages of simple operation, short process flow, low cost and environmental protection.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for recovering and preparing high-quality hydrochloric acid from waste gas of a phosgene reaction system comprises the following steps:
s1, adsorbing the waste gas in the phosgene reaction system by using water to obtain recovered hydrochloric acid;
and S2, adsorbing the recovered hydrochloric acid by adopting macroporous resin and activated carbon to obtain high-quality hydrochloric acid.
In the above method for recovering and preparing high-quality hydrochloric acid from the waste gas of the phosgene reaction system, in a further improvement, in step S2, the adsorption manner includes a first manner and a second manner;
the first method is as follows: adsorbing the recovered hydrochloric acid by using macroporous resin to obtain purified hydrochloric acid; adsorbing the purified hydrochloric acid by using activated carbon to obtain high-quality hydrochloric acid;
the second method comprises the following steps: adsorbing the recovered hydrochloric acid by using activated carbon to obtain purified hydrochloric acid; and adsorbing the purified hydrochloric acid by using macroporous resin to obtain high-quality hydrochloric acid.
The method for recovering and preparing the high-quality hydrochloric acid from the waste gas of the phosgene reaction system is further improved, and when the macroporous resin is adopted for adsorption, the recovered hydrochloric acid or the purified hydrochloric acid is introduced into an adsorption device filled with the macroporous resin.
In the method for recovering and preparing the high-quality hydrochloric acid from the waste gas of the phosgene reaction system, the recovered hydrochloric acid or the purified hydrochloric acid is introduced into an adsorption device filled with macroporous resin at the flow rate of 5 to 10 bv/h.
In the method for recovering and preparing the high-quality hydrochloric acid from the waste gas of the phosgene reaction system, the macroporous resin is poly (styrene-divinylbenzene) macroporous adsorption resin.
In the method for recovering and preparing the high-quality hydrochloric acid from the waste gas of the phosgene reaction system, the granularity of the poly (styrene-divinylbenzene) macroporous adsorption resin is further improved to be 0.315-1.250 mm; the pore diameter distribution range of the poly (styrene-divinylbenzene) macroporous absorption resin is
In the above method for recovering and preparing high-quality hydrochloric acid from the waste gas of the phosgene reaction system, in step S2, when activated carbon is used for adsorption, the recovered hydrochloric acid or the purified hydrochloric acid is introduced into an adsorption device filled with activated carbon.
In the above method for recovering and preparing high-quality hydrochloric acid from the waste gas of the phosgene reaction system, the recovered hydrochloric acid or purified hydrochloric acid is further improved at the flow rate of 5m3/h～10m3The reaction mixture is introduced into an adsorption unit containing activated carbon.
In the method for recovering and preparing the high-quality hydrochloric acid from the waste gas of the phosgene reaction system, the activated carbon is activated carbon fiber; the pore size distribution range of the activated carbon fiber is 100 nm-180 nm.
In the above method for recovering and preparing high-quality hydrochloric acid from the exhaust gas of the phosgene reaction system, the mass concentration of the high-quality hydrochloric acid in step S2 is further improved to 31% to 34%.
Compared with the prior art, the invention has the advantages that:
(1) the invention provides a method for recovering and preparing high-quality hydrochloric acid from waste gas of a phosgene reaction system, which comprises the steps of firstly adsorbing the waste gas in the phosgene reaction system by using water, dissolving hydrogen chloride hydrogen in the waste gas into the water to form recovered hydrochloric acid, further adsorbing the recovered hydrochloric acid by using macroporous resin and activated carbon, removing pungent phosgene smell in the recovered hydrochloric acid or purified hydrochloric acid and removing impurities (colors) in the purified hydrochloric acid to enable the recovered hydrochloric acid to become colorless and transparent, and obtaining the high-quality hydrochloric acid. The method has the advantages of simple operation, short process flow, low cost, environmental protection and the like, can prepare colorless industrial grade hydrochloric acid products meeting the national standard on the premise of ensuring lower preparation cost, and has high use value and high application prospect.
(2) According to the invention, the recovered hydrochloric acid or the purified hydrochloric acid is introduced into the adsorption device filled with the macroporous resin at the flow rate of 5-10 bv/h, so that the method has the advantages of ensuring sufficient contact time between the recovered hydrochloric acid or the purified hydrochloric acid and the macroporous resin, further improving the effect of removing the pungent phosgene odor in the recovered hydrochloric acid or the purified hydrochloric acid, simultaneously ensuring the effective use of the adsorption device and remarkably improving the treatment efficiency; the flow rate is higher than 10bv/h, so that the contact time of the hydrochloric acid and the macroporous adsorption resin is short, and a good impurity removal effect cannot be achieved; the flow rate is lower than 5bv/h, and the decoloring can be well realized, but the use efficiency of the device is influenced.
(3) In the present invention, the range of pore size distribution is adopted
The macroporous absorption resin of poly (styrene-divinylbenzene) can absorb the wastewater effectively, and the macroporous absorption resin has the advantage that the macroporous absorption resin can absorb the wastewater effectively and occupies most of the wastewater with the diameter
The colored impurities in the process are removed, so that the impurity removal effect is further improved, and hydrochloric acid with higher quality is obtained.
(4) In the present invention, the recovered hydrochloric acid or the purified hydrochloric acid is supplied at a flow rate of 5m3/h～10m3The method has the advantages that sufficient contact time is ensured between the recovered hydrochloric acid or the purified hydrochloric acid and the macroporous resin, the decoloring effect on the recovered hydrochloric acid or the purified hydrochloric acid is further improved, the effective use of the adsorption device can be ensured, and the treatment efficiency is obviously improved; and a flow velocity higher than 10m3H, then hydrochloric acid and macroporous absorptionThe contact time of the attached resin is short, and a good impurity removal effect cannot be achieved; flow velocity lower than 5m3However, the decolorization efficiency is affected although the decolorization is excellent.
(5) According to the invention, the activated carbon fiber with the pore size distribution range of 100 nm-180 nm is adopted for adsorption, so that the activated carbon can effectively adsorb most of colored impurities with the diameter of 100 nm-180 nm in the wastewater, the impurity removal effect is further improved, and hydrochloric acid with higher quality is obtained.
Drawings
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention.
FIG. 1 is a flow chart showing the process for recovering and preparing high-quality hydrochloric acid from the exhaust gas of a phosgene reaction system in examples 1 to 3 according to the present invention.
Detailed Description
The invention is further described below with reference to the drawings and specific preferred embodiments of the description, without thereby limiting the scope of protection of the invention.
The materials and equipment used in the following examples are commercially available. In the examples of the present invention, unless otherwise specified, the processes used were conventional processes, the equipment used were conventional equipment, and the data obtained were average values of three or more experiments.
Example 1:
a method for recovering and preparing high-quality hydrochloric acid from waste gas of a phosgene reaction system is shown in a process flow diagram of figure 1 and comprises the following steps:
(1) water adsorption: and absorbing the waste gas (namely the waste gas of the phosgene reaction system) in the o-hydroxybenzonitrile reaction system by water to obtain the recovered hydrochloric acid. And treating the residual waste gas by using an alkali liquor tower.
(2) Resin adsorption: the recovered hydrochloric acid obtained in the step (1) passes through a macroporous adsorption resin (with the granularity of 0.315mm and the pore diameter) filled with poly (styrene-divinylbenzene) at the flow rate of 8bv/h
) The adsorption apparatus of (1) removes the odor of the irritating phosgene in the recovered hydrochloric acid to obtain the purified hydrochloric acid.
(3) Adsorption by activated carbon fiber: the purified hydrochloric acid is added at 8m3Passing through an adsorption device with activated carbon fiber (aperture distribution range of 100nm) at a flow rate of/h, and adsorbing and decolorizing to make the product colorless and transparent to obtain high-quality hydrochloric acid product.
The obtained high-quality hydrochloric acid product was tested and analyzed, and the results are shown in table 1.
TABLE 1 data of the examination of the high quality hydrochloric acid product obtained in example 1 of the present invention
| Item | Qualified product | Example 1 |
| Mass fraction (%) of total acidity of not less than | 31 | 31.5 |
| The mass fraction (%) of iron is less than or equal to | 0.01 | 0.0001 |
| The mass fraction (%) of the burning residue is not more than | 0.15 | 0.15 |
| Mass fraction (%) of free chlorine is less than or equal to | 0.01 | 0.005 |
| The mass fraction (%) of arsenic is less than or equal to | 0.0001 | 0.00002 |
| Sulfate with w/% > less than or equal to | 0.05 | 0.02 |
Example 2:
a method for recovering and preparing high-quality hydrochloric acid from waste gas of a phosgene reaction system is shown in a process flow diagram of figure 1 and comprises the following steps:
(1) water adsorption: and absorbing the waste gas (namely the waste gas of the phosgene reaction system) in the o-hydroxybenzonitrile reaction system by water to obtain the recovered hydrochloric acid.
(2) Resin adsorption: the recovered hydrochloric acid obtained in the step (1) passes through a macroporous adsorption resin (with the particle size of 0.815mm and the pore diameter) filled with poly (styrene-divinylbenzene) at the flow rate of 8bv/h
) The adsorption apparatus of (1) removes the odor of the irritating phosgene in the recovered hydrochloric acid to obtain the purified hydrochloric acid.
(3) Adsorption by activated carbon fiber: the purified hydrochloric acid is added at 8m3The flow rate of the solution/h passes through an adsorption device provided with activated carbon fibers (the aperture distribution range is 140nm) to be adsorbed and decolored, so that the product is colorless and transparent, and a high-quality hydrochloric acid product is obtained.
The obtained high quality hydrochloric acid product was tested and analyzed, and the results are shown in table 2.
Table 2 test data of high quality hydrochloric acid product prepared in example 2 of the present invention
| Item | Qualified product | Example 2 |
| Mass fraction (%) of total acidity of not less than | 31 | 31 |
| The mass fraction (%) of iron is less than or equal to | 0.01 | 0.0001 |
| The mass fraction (%) of the burning residue is not more than | 0.15 | 0.15 |
| Mass fraction (%) of free chlorine is less than or equal to | 0.01 | 0.001 |
| The mass fraction (%) of arsenic is less than or equal to | 0.0001 | 0.000002 |
| Sulfate with w/% > less than or equal to | 0.05 | 0.01 |
Example 3:
a method for recovering and preparing high-quality hydrochloric acid from waste gas of a phosgene reaction system is shown in a process flow diagram of figure 1 and comprises the following steps:
(1) water adsorption: and absorbing the waste gas (namely the waste gas of the phosgene reaction system) in the o-hydroxybenzonitrile reaction system by water to obtain the recovered hydrochloric acid.
(2) Resin adsorption: the recovered hydrochloric acid obtained in the step (1) passes through a macroporous adsorption resin (with the granularity of 1.250mm and the pore diameter) filled with poly (styrene-divinylbenzene) at the flow rate of 10bv/h
) The adsorption apparatus of (1) removes the odor of the irritating phosgene in the recovered hydrochloric acid to obtain the purified hydrochloric acid.
(3) Adsorption by activated carbon fiber: the purified hydrochloric acid is added at a concentration of 10m3The flow rate of the solution/h passes through an adsorption device provided with activated carbon fibers (the aperture distribution range is 180nm), and the solution is adsorbed and decolored, so that the product is colorless and transparent, and a high-quality hydrochloric acid product is obtained.
The obtained high quality hydrochloric acid product was tested and analyzed, and the results are shown in table 3.
TABLE 3 data of the high quality hydrochloric acid product obtained in example 3 of the present invention
| Item | Qualified product | Example 3 |
| Mass fraction (%) of total acidity of not less than | 31 | 34 |
| The mass fraction (%) of iron is less than or equal to | 0.01 | 0.0001 |
| The mass fraction (%) of the burning residue is not more than | 0.15 | 0.15 |
| Mass fraction (%) of free chlorine is less than or equal to | 0.01 | 0.005 |
| The mass fraction (%) of arsenic is less than or equal to | 0.0001 | 0.00002 |
| Sulfate with w/% > less than or equal to | 0.05 | 0.02 |
As can be seen from tables 1-3, the hydrochloric acid obtained after the treatment by the method of the invention can meet the national industrial grade hydrochloric acid index requirements. Meanwhile, the preparation cost of the high-quality hydrochloric acid in the examples 1 to 3 is 9.4 to 10.0 yuan/ton, and the process cost is 40 to 50 yuan/ton when the hydrochloric acid is recovered and purified by steam and calcium chloride. Therefore, the method has the advantages of simple operation, short process flow, low cost, environmental protection and the like, can prepare colorless industrial grade hydrochloric acid products meeting the national standard on the premise of ensuring lower preparation cost, and has high use value and high application prospect.
Example 4:
a method for recovering and preparing high-quality hydrochloric acid from waste gas of a phosgene reaction system comprises the following steps:
(1) water adsorption: and absorbing the waste gas (namely the waste gas of the phosgene reaction system) in the o-hydroxybenzonitrile reaction system by water to obtain the recovered hydrochloric acid.
(2) Adsorption by activated carbon fiber: the recovered hydrochloric acid obtained in the step (1) is added at a concentration of 10m3H ofPassing through an adsorption device equipped with activated carbon fiber (aperture distribution range of 180nm) at a flow rate, adsorbing and decolorizing to make the product colorless and transparent, and obtaining purified hydrochloric acid.
(3) Resin adsorption: purified hydrochloric acid is passed through a macroporous adsorbent resin (granularity 1.250mm, aperture) filled with poly (styrene-divinylbenzene) at a flow rate of 10bv/h
) The adsorption device removes the odor of the irritating phosgene in the recovered hydrochloric acid to obtain a high-quality hydrochloric acid product.
The obtained high quality hydrochloric acid product was tested and analyzed, and the results are shown in table 4.
Table 4 test data of high quality hydrochloric acid product obtained in example 4 of the present invention
| Item | Qualified product | Example 3 |
| Mass fraction (%) of total acidity of not less than | 31 | 34 |
| The mass fraction (%) of iron is less than or equal to | 0.01 | 0.0002 |
| The mass fraction (%) of the burning residue is not more than | 0.15 | 0.15 |
| Mass fraction (%) of free chlorine is less than or equal to | 0.01 | 0.005 |
| The mass fraction (%) of arsenic is less than or equal to | 0.0001 | 0.00002 |
| Sulfate with w/% > less than or equal to | 0.05 | 0.02 |
As can be seen from Table 4, the hydrochloric acid obtained by the treatment of the method of the present invention can meet the national industrial grade hydrochloric acid index requirements.
The above examples are merely preferred embodiments of the present invention, and the scope of the present invention is not limited to the above examples. All technical schemes belonging to the idea of the invention belong to the protection scope of the invention. It should be noted that modifications and embellishments within the scope of the invention may be made by those skilled in the art without departing from the principle of the invention, and such modifications and embellishments should also be considered as within the scope of the invention.
Claims (10)
1. A method for recovering and preparing high-quality hydrochloric acid from waste gas of a phosgene reaction system is characterized by comprising the following steps:
s1, adsorbing the waste gas in the phosgene reaction system by using water to obtain recovered hydrochloric acid;
and S2, adsorbing the recovered hydrochloric acid by adopting macroporous resin and activated carbon to obtain high-quality hydrochloric acid.
2. The method for recovering and producing high-quality hydrochloric acid from an exhaust gas of a phosgene reaction system according to claim 1, wherein in step S2, the adsorption manner includes a first manner and a second manner;
the first method is as follows: adsorbing the recovered hydrochloric acid by using macroporous resin to obtain purified hydrochloric acid; adsorbing the purified hydrochloric acid by using activated carbon to obtain high-quality hydrochloric acid;
the second method comprises the following steps: adsorbing the recovered hydrochloric acid by using activated carbon to obtain purified hydrochloric acid; and adsorbing the purified hydrochloric acid by using macroporous resin to obtain high-quality hydrochloric acid.
3. The method for recovering and preparing high-quality hydrochloric acid from the exhaust gas of a phosgene reaction system as claimed in claim 2, wherein, when the macroporous resin is used for adsorption, the recovered hydrochloric acid or the purified hydrochloric acid is introduced into an adsorption device containing the macroporous resin.
4. The method for recovering and preparing high-quality hydrochloric acid from the exhaust gas of a phosgene reaction system according to claim 3, wherein the recovered hydrochloric acid or the purified hydrochloric acid is introduced into an adsorption device equipped with a macroporous resin at a flow rate of 5 to 10 bv/h.
5. The method for recovering and preparing high-quality hydrochloric acid from the waste gas of the phosgene reaction system according to claim 4, wherein the macroporous resin is poly (styrene-divinylbenzene) macroporous adsorption resin.
6. The method for recovering and preparing high-quality hydrochloric acid from the waste gas of a phosgene reaction system according to claim 5, wherein the particle size of the poly (styrene-divinylbenzene) macroporous adsorption resin is 0.315mm to 1.250 mm; the pore diameter distribution range of the poly (styrene-divinylbenzene) macroporous absorption resin is
7. The method for recovering and preparing high-quality hydrochloric acid from the exhaust gas of a phosgene reaction system as claimed in any one of claims 1 to 6, wherein in step S2, when activated carbon is used for adsorption, the recovered hydrochloric acid or the purified hydrochloric acid is introduced into an adsorption apparatus containing activated carbon.
8. The method for recovering and preparing high-quality hydrochloric acid from the exhaust gas of a phosgene reaction system as claimed in claim 7, wherein the recovered hydrochloric acid or the purified hydrochloric acid is used at a flow rate of 5m3/h～10m3The reaction mixture is introduced into an adsorption unit containing activated carbon.
9. The method for recovering and preparing high-quality hydrochloric acid from the exhaust gas of a phosgene reaction system as claimed in claim 8, wherein the activated carbon is activated carbon fiber; the pore size distribution range of the activated carbon fiber is 100 nm-180 nm.
10. The method for recovering and preparing high-quality hydrochloric acid from the exhaust gas of a phosgene reaction system according to any one of claims 1 to 6, wherein the mass concentration of the high-quality hydrochloric acid in step S2 is 31% to 34%.
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| CN112456441A (en) * | 2020-11-05 | 2021-03-09 | 江苏永葆环保科技有限公司 | Purification pretreatment method of chemical byproduct hydrochloric acid |
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Application publication date: 20201020 |