CN106268215A - The manufacture method of a kind of desulfurizing agent and prepared desulfurizing agent - Google Patents
The manufacture method of a kind of desulfurizing agent and prepared desulfurizing agent Download PDFInfo
- Publication number
- CN106268215A CN106268215A CN201610788650.6A CN201610788650A CN106268215A CN 106268215 A CN106268215 A CN 106268215A CN 201610788650 A CN201610788650 A CN 201610788650A CN 106268215 A CN106268215 A CN 106268215A
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- CN
- China
- Prior art keywords
- desulfurizing agent
- manufacture method
- butylene succinate
- poly butylene
- weight portion
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/48—Sulfur compounds
- B01D53/50—Sulfur oxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/48—Sulfur compounds
- B01D53/52—Hydrogen sulfide
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/81—Solid phase processes
Abstract
The invention belongs to chemical field, relate to the manufacture method of a kind of desulfurizing agent, comprise the steps, ferrum oxide, ferrous sulfate, fluorite and magnesium chloride are mixed by (1)；(2) in the mixture that step (1) obtains, add sodium borate and poly butylene succinate, mix at 90 DEG C 120 DEG C, then maintenance 20 25 hours, dry, roasting；(3) calcining matter that step (2) obtains is put into constant temperature dipping in the poly butylene succinate of 120 200 DEG C, then dries, cool down.The invention still further relates to the desulfurizing agent that described method obtains.Sulfur capacity and the desulfurization precision of inventive desulfurization agent are higher, crushing strength is higher, specific surface area is bigger, improve the desulfuration efficiency in industrial application.
Description
Technical field
The invention belongs to chemical field, be specifically related to the manufacture method of a kind of desulfurizing agent, further relate to obtained by the method
Desulfurizing agent.
Background technology
In commercial production a lot of in the case of all can produce sulfide, such as coal or oil and the industrial chemicals produced thereof
In, the waste water of commercial production discharge, waste gas all contains sulfide.Sulfide is mainly derived from the sulfur material contained in raw material,
Sulfur material reacts in industrial processes and changes into sulfide, thus discharges.Sulfide particularly hydrogen sulfide, titanium dioxide
Sulfur etc. can frequently result in the catalyst poisoning inactivation produced in workshop section, and directly discharges, also containing the waste water of sulfide, waste gas
Easily pollute environment, cause person poultry poisoning.
Desulfurizing agent is a kind of for removing the medicament of sulfide in raw material, waste water, waste gas or unclassified stores.Owing to reducing sulfur
U content is conducive to commercial production and environmental conservation, and therefore researcher gives more concern for the research and development of desulfurizing agent.
Current desulfurizing agent kind includes solid base/liquid base desulfurizing agent, activated carbon desulphurization agent, molecular sieve carried metal desulfurization agent, ferrum
Fimily desulfurizing agent, manganese systems desulfurizing agent, many composite oxide of metal desulfurizing agent etc..Study through for many years, although desulfurizing agent kind is more come
The abundantest, desulfurization performance there has also been and is greatly improved, but existing desulfurizing agent Sulfur capacity and desulfurization precision are the most relatively low, it is difficult to
Meet commercial production to desulfuration efficiency and the requirement of economic performance.
Still need at present a kind of Sulfur capacity and the higher desulfurizing agent of desulfurization precision, to improve desulfuration efficiency, meet industry needs.
Summary of the invention
The inventors found that the manufacture method of a kind of desulfurizing agent, obtained desulfurizing agent Sulfur capacity is high, desulfurization essence
Degree is high, crushing strength is high, specific surface area is big, substantially increases the desulfuration efficiency in industrial application.
First aspect present invention relates to the manufacture method of a kind of desulfurizing agent, comprises the steps,
(1) ferrum oxide, ferrous sulfate, fluorite and magnesium chloride are mixed；
(2) in the mixture that step (1) obtains, sodium borate and poly butylene succinate are added, at 90 DEG C-120 DEG C
Mixing, then maintenance 20-25 hour, dry, roasting；Preferably, 90-110 DEG C, 90 DEG C, 95 DEG C, 100 DEG C, 105 DEG C, 110 DEG C,
Mix homogeneously at 115 DEG C or 120 DEG C；Preferably, curing time is 20 hours, 22 hours, 23 hours or 25 hours；
(3) calcining matter that step (2) obtains is put into constant temperature dipping in the poly butylene succinate of 120-200 DEG C, then
Dry, cool down；Preferably calcining matter is put into 120-160 DEG C, 120 DEG C, 130 DEG C, 140 DEG C, 150 DEG C, 160 DEG C, 170 DEG C,
Constant temperature dipping in the poly butylene succinate of 180 DEG C, 190 DEG C or 200 DEG C.
In any embodiment of first aspect present invention, in step (3), the temperature of constant temperature dipping is poly-fourth in step (3)
The temperature of succinate adipate.
In any embodiment of first aspect present invention, the addition of described ferrum oxide be 40-53 weight portion (preferably
40,50 or 53 weight portion), the addition of described ferrous sulfate is 20-35 weight portion (preferably 20,28 or 35 weight portion), institute
The addition stating fluorite is 15-20 weight portion (preferably 15,18 or 20 weight portion), and the addition of described magnesium chloride is 8-14 weight
Amount part (preferably 8,12 or 14 weight portion).
In any embodiment of first aspect present invention, described ferrum oxide, the particle diameter of fluorite be 600-1000 μm (preferably
600,700,800,850,900 or 1000 μm).
In any embodiment of first aspect present invention, described ferrous sulfate, the particle diameter of magnesium chloride are 200-500 μm
(preferably 200,300,350,400 or 500 μm).
The ferrum oxide of above-mentioned particle diameter, ferrous sulfate, fluorite and magnesium chloride mixing are more uniform.
In any embodiment of first aspect present invention, the addition of described sodium borate be 5-13 weight portion (preferably
5,9 or 13 weight portion), the addition of the described poly butylene succinate in step (2) be 7-15 weight portion (preferably 7,8,
10 or 15 weight portions).
Sodium borate contributes to making poly butylene succinate and ferrum oxide, ferrous sulfate, fluorite and the mixture of magnesium chloride
Uniformly merge.
In any embodiment of first aspect present invention, described in step (2), the particle diameter of poly butylene succinate is
300-800 μm, preferably 300 μm, 400 μm, 500 μm, 700 μm or 800 μm.The poly butylene succinate of this particle size range is more
Easy and ferrum oxide, ferrous sulfate, fluorite and magnesium chloride mixture merges uniformly.
In any embodiment of first aspect present invention, the temperature of maintenance is 80-100 DEG C；Be preferably 80 DEG C, 90 DEG C,
95 DEG C or 100 DEG C.
In any embodiment of first aspect present invention, the drying temperature in step (2) and/or step (3) is 120-
150℃；Preferably, the drying temperature in step (2) and/or step (3) is 120 DEG C, 130 DEG C, 140 DEG C or 150 DEG C.
The purpose dried in step (2) and/or step (3) is to reduce water content, and moisture mostlys come from raw material.
In any embodiment of first aspect present invention, sintering temperature is 200-250 DEG C；Be preferably 200 DEG C, 210 DEG C,
220 DEG C, 225 DEG C, 230 DEG C, 240 DEG C or 250 DEG C.
In any embodiment of first aspect present invention, roasting time is 0.5-2 hour, preferably 0.5,1,1.5 or 2
Hour.
In roasting process, under sodium borate participates in (may be for catalytic action), poly butylene succinate occurs chemistry to become
Change.
In any embodiment of first aspect present invention, the addition of poly butylene succinate described in step (3)
For 20-45 weight portion；It is preferably 30-45 weight portion, 20 weight portions, 30 weight portions, 40 weight portions or 45 weight portions.
In any embodiment of first aspect present invention, dip time is 8-12 hour；It is preferably 8 hours, 10 hours
Or 12 hours.Dipping makes poly butylene succinate and ferrum oxide, ferrous sulfate, fluorite and magnesium chloride granules carry out the degree of depth to melt
Close.
Poly-succinic acid-butanediol in any embodiment of first aspect present invention, in step (2) and/or step (3)
Number-average molecular weight Mn of ester is 1 × 105～2 × 105；Preferably, the poly-succinic acid-butanediol in step (2) and/or step (3)
Number-average molecular weight Mn of ester is 1 × 105、1.5×105Or 2 × 105。
Second aspect present invention relates to the desulfurizing agent that above-mentioned manufacture method obtains.
The beneficial effect that the present invention obtains:
1, the Sulfur capacity of the desulfurizing agent that the desulfurizing agent manufacture method of the present invention obtains is high, desulfurization precision is high, crushing strength is high,
Specific surface area is big, improves the desulfuration efficiency in industrial application.
2, the present invention prepares desulfurizing agent using poly butylene succinate as one of raw material, improves the performance of desulfurizing agent.
3, the present invention adds sodium borate when making desulfurizing agent, it is possible to increase poly butylene succinate merges with other raw materials
Uniformity, and sodium borate can be catalyzed poly butylene succinate and chemical change occurs in roasting process.
Detailed description of the invention
In order to make present disclosure be more likely to be clearly understood, below in conjunction with the specific embodiment of the present invention to this
Bright it is described in further detail, but specific embodiment itself does not cause limiting the scope of the invention.
Embodiment 1
400g ferrum oxide, 200g ferrous sulfate, 150g fluorite and 80g magnesium chloride mix homogeneously, magnesium chloride and sulphuric acid is sub-
The particle diameter of ferrum be the particle diameter of 200-400 μm, fluorite and ferrum oxide be 600-800 μm.50g boric acid is added in the mixture obtained
Sodium and 70g poly butylene succinate, mix homogeneously at 90 DEG C-100 DEG C, the particle diameter of poly butylene succinate is 300-
500 μm, then maintenance 20 hours at 80-90 DEG C, with 120 DEG C of drying, obtain compound A, and then compound A roasts at 200 DEG C
Burn 2 hours, obtain calcining matter A.The calcining matter obtained is put into constant temperature dipping 8 in the 200g poly butylene succinate of 120 DEG C
Hour, then in 140 DEG C of drying, cooling, obtain desulfurizing agent 1.Number-average molecular weight Mn of the poly butylene succinate used is 1.5
×105-2×105。
Embodiment 2
500g ferrum oxide, 280g ferrous sulfate, 180g fluorite and 120g magnesium chloride mix homogeneously, magnesium chloride and sulphuric acid is sub-
The particle diameter of ferrum be the particle diameter of 300-400 μm, fluorite and ferrum oxide be 700-900 μm.90g boric acid is added in the mixture obtained
Sodium and 100g poly butylene succinate, mix homogeneously at 110 DEG C-120 DEG C, the particle diameter 400-of poly butylene succinate
600 μm, then maintenance 23 hours at 90-95 DEG C, with 140 DEG C of drying, then roasting 1 hour at 230 DEG C.The roasting that will obtain
Thing is put into constant temperature in the 300g poly butylene succinate of 130 DEG C and is impregnated 12 hours, then 150 DEG C of drying, cool down, obtain desulfurization
Agent 2.Number-average molecular weight Mn of the poly butylene succinate used is 1 × 105-1.5×105。
Embodiment 3
530g ferrum oxide, 350g ferrous sulfate, 200g fluorite and 140g magnesium chloride mix homogeneously, magnesium chloride and sulphuric acid is sub-
The particle diameter of ferrum be the particle diameter of 400-500 μm, fluorite and ferrum oxide be 900-1000 μm.130g boron is added in the mixture obtained
Acid sodium and 150g poly butylene succinate, mix homogeneously at 110 DEG C-120 DEG C, the particle diameter 700-of poly butylene succinate
800 μm, then maintenance 25 hours at 95-100 DEG C, with 150 DEG C of drying, then roasting 0.5 hour at 250 DEG C.By obtain
Calcining matter is put into constant temperature in the 450g poly butylene succinate of 140 DEG C and is impregnated 10 hours, then 150 DEG C of drying, cool down, obtain
Desulfurizing agent 3.Number-average molecular weight Mn of the poly butylene succinate used is 1 × 105-1.5×105。
Comparative example 1
400g ferrum oxide, 200g ferrous sulfate, 150g fluorite and 80g magnesium chloride are added 20g water mix homogeneously, magnesium chloride and
The particle diameter of ferrous sulfate be the particle diameter of 200-400 μm, fluorite and ferrum oxide be 600-800 μm, then maintenance 20 is little at 80-90 DEG C
Time, with 120 DEG C of drying, then roasting 2 hours at 200 DEG C, cool down calcining matter, obtain desulfurizing agent A.
Comparative example 2
400g ferrum oxide, 200g ferrous sulfate, 150g fluorite and 80g magnesium chloride mix homogeneously, magnesium chloride and sulphuric acid is sub-
The particle diameter of ferrum be the particle diameter of 200-400 μm, fluorite and ferrum oxide be 600-800 μm.The poly-fourth of 70g is added in the mixture obtained
Succinate adipate, mix homogeneously at 90 DEG C-100 DEG C, the particle diameter of poly butylene succinate is 300-500 μm, then at 80-
Maintenance 20 hours at 90 DEG C, with 120 DEG C of drying, obtain compound B.By compound B roasting 2 hours at 200 DEG C, obtain roasting
Thing B.Number-average molecular weight Mn of the poly butylene succinate used is 1.5 × 105-2×105。
Experimental example 1 desulfurization precision, Sulfur capacity and physical property
1, desulfurization precision
Unstripped gas is set for containing 5000ppmH2The nitrogen of S, each 3g of desulfurizing agent 1-3, A of Example 1-3 and comparative example 1,
At normal pressure (usually 1 atmospheric pressure), carrying out repeatedly desulfurization test between 10-45 DEG C respectively, gas air speed is 2000h-1。
Finally recording: under each temperature conditions, unstripped gas is after desulfurizing agent 1-3 processes, and outlet total sulfur is below
0.01ppm；Unstripped gas is after desulfurizing agent A processes, and outlet total sulfur is about 0.08ppm.Therefore, the desulfurizing agent 1-3's of the present invention is de-
Sulfur precision is higher than desulfurizing agent A.
2, Sulfur capacity and physical property
Desulfurizing agent 1-3, A of Example 1-3 and comparative example 1 make sample, measure Sulfur capacity respectively.Take sample 100g, 10
DEG C-45 DEG C, under normal pressure (usually 1 atmospheric pressure), with containing H2S is that the Standard Gases of 40000ppm is evaluated and tested.Qualitative detection, can be certainly
Join silver nitrate solution outlet sulfur is detected；Detection by quantitative, can use domestic WK-2C comprehensive Microcoulomb instrument (Jiangsu electroanalysis
Instrument plant) detect, the detection limit of this instrument is 0.2ppm, and result is as shown in table 1.
Table 1
| Test event | Desulfurizing agent 1 | Desulfurizing agent 2 | Desulfurizing agent 3 | Desulfurizing agent A |
| Sulfur capacity | 79.6% | 80.5% | 81.0% | 44.3% |
Visible, the Sulfur capacity of inventive desulfurization agent 1-3 is far longer than desulfurizing agent A.
After measured, the crushing strength of inventive desulfurization agent 1-3 is more than 110N/cm, and specific surface area is 80-120m2/g；De-
The crushing strength of sulfur agent A is 40N/cm, and specific surface area is 50-60m2/g.The crushing strength of inventive desulfurization agent 1-3 and ratio
Surface area is above desulfurizing agent A.
Experimental example 2: mixture uniformity and calcining matter chemical change
1, mixture uniformity
The compound A-B of embodiment 1, comparative example 2 is detected.
The random 10g that respectively takes compound A-B, as sample, observes with microscope, it can be observed that: bigger in compound B
Granule (may be considered merge formed granule) substantially concentrate on central authorities, do not scatter；And it is bigger in compound A sample
Granule (may be considered merge formed granule) in the most all there being distribution, disperse the most uniform.Therefore, add sodium borate to have
Help make poly butylene succinate merge equably with other raw materials, then it is observed that the bulky grain being fused into throughout
It is uniformly distributed.
2, calcining matter chemical change
Compound A-B and calcining matter A-B to embodiment 1, comparative example 2 uses the Nexus 670 of Nicolet company of the U.S.
Type Fourier transformation infrared spectrometer detects under similarity condition.Found that: compound B and the infrared light of calcining matter B
Spectrum extremely approximates；The infrared spectrum difference of calcining matter A and compound A is relatively big, except the ester group absworption peak in calcining matter A spectrogram subtracts
Outside weak, the infrared spectrum of calcining matter A also spectrogram than compound A is many 3 absworption peaks.Add sodium borate and contribute to poly-succinic
Chemical change is there is in butanediol ester in roasting process.
Obviously, above-described embodiment is only for clearly demonstrating example, and not restriction to embodiment.Right
For those of ordinary skill in the field, can also make on the basis of the above description other multi-form change or
Variation.Here without also cannot all of embodiment be given exhaustive.And the obvious change thus extended out or
Change among still in the protection domain of the invention.
Claims (10)
1. a manufacture method for desulfurizing agent, comprises the steps,
(1) ferrum oxide, ferrous sulfate, fluorite and magnesium chloride are mixed；
(2) in the mixture that step (1) obtains, sodium borate and poly butylene succinate are added, mixed at 90 DEG C-120 DEG C
Close, then maintenance 20-25 hour, dry, roasting；
(3) calcining matter that step (2) obtains is put into constant temperature in the poly butylene succinate of 120-200 DEG C impregnate, then dry,
Cool down.
Manufacture method the most according to claim 1, wherein, the addition of described ferrum oxide is 40-53 weight portion, described sulfur
The addition of acid ferrous iron is 20-35 weight portion, and the addition of described fluorite is 15-20 weight portion, the addition of described magnesium chloride
For 8-14 weight portion.
Manufacture method the most according to claim 1, wherein, the addition of described sodium borate is 5-13 weight portion, step (2)
Described in the addition of poly butylene succinate be 7-15 weight portion.
Manufacture method the most according to claim 1, wherein, the temperature of maintenance is 80 DEG C-100 DEG C.
Manufacture method the most according to claim 1, wherein, the drying temperature in step (2) and/or step (3) is 120-
150℃。
Manufacture method the most according to claim 1, wherein, sintering temperature is 200-250 DEG C.
Manufacture method the most according to claim 1, wherein, the addition of poly butylene succinate described in step (3)
For 20-45 weight portion.
Manufacture method the most according to claim 1, wherein, dip time is 8-12 hour.
9. according to the manufacture method according to any one of claim 1-8, wherein, the poly-fourth in step (2) and/or step (3)
Number-average molecular weight Mn of succinate adipate is 1 × 105～2 × 105。
10. the desulfurizing agent obtained by the manufacture method according to any one of claim 1-9.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610788650.6A CN106268215A (en) | 2016-08-30 | 2016-08-30 | The manufacture method of a kind of desulfurizing agent and prepared desulfurizing agent |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610788650.6A CN106268215A (en) | 2016-08-30 | 2016-08-30 | The manufacture method of a kind of desulfurizing agent and prepared desulfurizing agent |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1193042A (en) * | 1997-03-10 | 1998-09-16 | 王保行 | High-energy sweetening coal-saving agent |
| CN1287628A (en) * | 1998-11-05 | 2001-03-14 | Ldt激光展示技术公司 | Projection system with projector and deflection mirror |
| CN102851090A (en) * | 2012-09-03 | 2013-01-02 | 杭州萧山管道燃气发展有限公司 | Biogas dry-type filtering desulphurization system and preparation method thereof |
-
2016
- 2016-08-30 CN CN201610788650.6A patent/CN106268215A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1193042A (en) * | 1997-03-10 | 1998-09-16 | 王保行 | High-energy sweetening coal-saving agent |
| CN1287628A (en) * | 1998-11-05 | 2001-03-14 | Ldt激光展示技术公司 | Projection system with projector and deflection mirror |
| CN102851090A (en) * | 2012-09-03 | 2013-01-02 | 杭州萧山管道燃气发展有限公司 | Biogas dry-type filtering desulphurization system and preparation method thereof |
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