CN105130928A - Method for removing trace oxygen from hydrogen peroxide propylene oxide process mixing gas - Google Patents

Method for removing trace oxygen from hydrogen peroxide propylene oxide process mixing gas Download PDF

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Publication number
CN105130928A
CN105130928A CN201510496036.8A CN201510496036A CN105130928A CN 105130928 A CN105130928 A CN 105130928A CN 201510496036 A CN201510496036 A CN 201510496036A CN 105130928 A CN105130928 A CN 105130928A
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propylene
oxygen
gas mixture
propylene oxide
hydrogen peroxide
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CN105130928B (en
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文松
姜杰
孙冰
张铁
赵磊
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China Petroleum and Chemical Corp
Sinopec Qingdao Safety Engineering Institute
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China Petroleum and Chemical Corp
Sinopec Qingdao Safety Engineering Institute
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D303/00—Compounds containing three-membered rings having one oxygen atom as the only ring hetero atom
    • C07D303/02—Compounds containing oxirane rings
    • C07D303/04—Compounds containing oxirane rings containing only hydrogen and carbon atoms in addition to the ring oxygen atoms
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D301/00—Preparation of oxiranes
    • C07D301/02—Synthesis of the oxirane ring
    • C07D301/03—Synthesis of the oxirane ring by oxidation of unsaturated compounds, or of mixtures of unsaturated and saturated compounds
    • C07D301/12—Synthesis of the oxirane ring by oxidation of unsaturated compounds, or of mixtures of unsaturated and saturated compounds with hydrogen peroxide or inorganic peroxides or peracids

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Catalysts (AREA)

Abstract

The present invention relates to a method for removing trace oxygen from hydrogen peroxide propylene oxide process mixing gas. A purpose of the present invention is mainly to solve the problems of easy explosion and high nitrogen consumption of the propylene buffer tank in the prior art. According to the present invention, the method for removing trace oxygen from hydrogen peroxide propylene oxide process mixing gas is used, a deoxygenation reactor is arranged between a circulating propylene compressor and a propylene buffer tank, process mixing gas and hydrogen are mixed through a gas mixer, the mixed gas enters the deoxygenation reactor and contacts a catalyst, the catalyst can make oxygen and hydrogen be subjected to a reaction while make hydrogen and propylene be not subjected to a reaction, and the deoxygenation reactor outlet material enters the propylene buffer tank. With the technical scheme, the problems in the prior art are well solved. The method of the present invention can be used for the deoxygenation of the hydrogen peroxide propylene oxide process mixing gas.

Description

Remove the method for hydrogen peroxide legal system propylene oxide process gas mixture micro amount of oxygen
Technical field
The present invention relates to a kind of method removing hydrogen peroxide legal system propylene oxide process gas mixture micro amount of oxygen.
Background technology
Propylene oxide is very important organic compound raw material, is the third-largest propylene analog derivative being only second to polypropylene and vinyl cyanide.Propylene oxide has two large main applications, and one is for the production of propylene dibasic alcohol, and one is used to produce polyvalent alcohol.Polyvalent alcohol is the main raw material producing urethane, and polyurethane material purposes widely, can replace rubber, nylon etc. for multiple occasion, as lagging material, coating, sizing agent, foam, elastomerics etc.And propylene dibasic alcohol is the main raw of production cosmetic, wetting Agent for Printing Inks, deicing fluid, lubricating fluid additive.
Hydrogen peroxide legal system propylene oxide (hydrogeneperoxidepropyleneoxide) technique is a kind of novel Synthesis of Propylene Oxide, this technique is using hydrogen peroxide and propylene as raw material, reaction generates propylene oxide and water, compare conventional epoxy oxide production process, hydrogen peroxide legal system propylene oxide process has that clean environment firendly, Infrastructure are few, the advantage of no coupling product, but this technique also exists corresponding problem.Can there is decomposition in hydrogen peroxide in technological process, and the concentration of oxygen in circulation propylene is increased, and easily produces and fire operating mode, and then cause danger classes to raise in propylene surge tank.
CN201310076350.1 provides a kind of method of deoxidation of coalbed methane containing oxygen, it is characterized in that: coalbed methane containing oxygen and artificial coal gas are passed into and is equipped with in the reactor of catalyzer, under the effect of catalyzer, make the oxygen in the carbon monoxide in artificial coal gas and hydrogen and coal-seam gas carry out reacting and generate carbonic acid gas and water and reach the object removing oxygen.
Industrial in order to address this problem the method adopting nitrogen dilution or discharge torch, the method nitrogen consumption of nitrogen dilution is large, and the method propylene of discharge torch is wasted in a large number, and two kinds of methods all have impact on economic benefit.Therefore develop suitable deoxidization technique and deoxidation treatment carried out to this circulation propylene, to reduction plant energy consumption, increase economic efficiency significant.
Summary of the invention
Technical problem to be solved by this invention is the problem that in prior art, propylene surge tank easily fires, nitrogen consumption is large, provides a kind of method removing hydrogen peroxide legal system propylene oxide process gas mixture micro amount of oxygen newly.The method is used for, in the deoxidation of hydrogen peroxide legal system propylene oxide process gas mixture, having the advantage that propylene surge tank is not easy to blast, nitrogen consumption is little.
For solving the problem, the technical solution used in the present invention is as follows: a kind of method removing hydrogen peroxide legal system propylene oxide process gas mixture micro amount of oxygen, produce between the circulation propylene compressor of propylene oxide full scale plant and propylene surge tank at peroxide passivation and deoxidation reactor is set, the technique gas mixture of described full scale plant and hydrogen enter deoxidation reactor after gas mixer mixing, with catalyst exposure, deoxidation reactor outlet material enters propylene surge tank; Technique gas mixture pipeline before entering gas mixer arranges oxygen content analyser, and forms three with the feed valve on hydrogen pipeline and get two interlocked control, control the aperture of hydrogen feed valve; Establish oxygen content analyser at deoxidation reactor top, and form three with the control valve put on scare line at deoxidation reactor top and get two interlocked control, start interlocking when oxygen volume content is more than 5%, deoxidation reactor top gas mixture is disposed to torch; Propylene surge tank arranges oxygen content analyser, and forms three with the control valve put on scare line on propylene surge tank and get two interlocked control, start interlocking when oxygen volume content is more than 5%, the gas mixture of propylene surge tank is disposed to torch; Wherein, described catalyzer is Pd/ aluminum oxide, adopts the method preparation comprised the steps:
(1) by NaCl and PdCl 2be between 1.5 ~ 4, be made into chlorine palladium acid sodium solution with mol ratio;
(2) alumina supporter is joined in chlorine palladium acid sodium steeping fluid, steeping fluid is put into ultrasonic oscillation instrument and carry out ultrasonic oscillation dipping;
(3) ultrasonic oscillation dipping 2 ~ 8h, then by sample at room temperature ageing >=8h;
(4) sample is put into loft drier, under the temperature condition of >=80 DEG C, carry out drying;
(5) by dried sample in high temperature resistance furnace at 300 ~ 600 DEG C roasting >=2h;
(6) prepare sodium formate solution to reduce to palladium catalyst, reduction temperature is 70 ~ 100 DEG C, and the recovery time is >=2h, and the consumption of sodium formiate is 3 ~ 6 times of Palladium Content in Catalyst;
(7) reduced rear to reduction after palladium catalyst wash fully;
(8) catalyzer after washing is carried out drying under >=80 DEG C of conditions, obtain shaping Pd/ aluminium oxide catalyst.
In technique scheme, preferably, measure the oxygen content of deoxidation reactor import and outlet, calculate the DNA vaccine of catalyzer, the DNA vaccine of described catalyzer is greater than 90%.
In technique scheme, preferably, the reaction conditions of described deoxidation reactor is: 50 ~ 100 DEG C; 0 ~ 0.5MPa.
In technique scheme, preferably, in described catalyzer, the mass ratio of palladium and alumina supporter is 1 ‰ ~ 5 ‰.
In technique scheme, preferably, when the oxygen volume content at deoxidation reactor top is more than 1% alarm, after reporting to the police, operator need check hydrogen inlet, temperature of reaction and stop 1 and stay the time, and the activity of sampling and testing catalyzer.
The present invention can remove peroxide passivation and produce oxygen after propylene oxide reaction in gas mixture, adopt the oxygen concentration in effective catalyst reduction gas mixture, the inside oxygen level of propylene surge tank in technique is not exceeded standard, does not form the system of firing, the safety of effective guarantee device reaction system; Decrease simultaneously the consumption of nitrogen and oxygen too high time propylene row torch a large amount of wastes, improve economic benefit, achieve good technique effect.
Below by embodiment, the invention will be further elaborated, but be not limited only to the present embodiment.
Embodiment
[embodiment 1]
A kind of method removing hydrogen peroxide legal system propylene oxide process gas mixture micro amount of oxygen, produce between the circulation propylene compressor of propylene oxide full scale plant and propylene surge tank at peroxide passivation and deoxidation reactor is set, the technique gas mixture of described full scale plant and hydrogen enter deoxidation reactor after gas mixer mixing, with catalyst exposure, described catalyzer can make that oxygen and hydrogen react and propylene and hydrogen do not react, and deoxidation reactor outlet material enters propylene surge tank; Wherein, the technique gas mixture pipeline before entering gas mixer arranges oxygen content analyser, and form three with the feed valve on hydrogen pipeline and get two interlocked control, control the aperture of hydrogen feed valve, namely control the mol ratio of hydrogen and oxygen; Oxygen content analyser is established at deoxidation reactor top, and form three with the control valve put on scare line at deoxidation reactor top and get two interlocked control, when the oxygen volume content at deoxidation reactor top is more than 1% alarm, after reporting to the police, operator need check hydrogen inlet, temperature of reaction and the residence time, and the activity of sampling and testing catalyzer.Start interlocking when oxygen volume content is more than 5%, deoxidation reactor top gas mixture is disposed to torch; Propylene surge tank arranges oxygen content analyser, and forms three with the control valve put on scare line on propylene surge tank and get two interlocked control, start interlocking when oxygen volume content is more than 5%, the gas mixture of propylene surge tank is disposed to torch.
Described catalyzer is Pd/ aluminum oxide, adopts the method preparation comprised the steps:
(1) by NaCl and PdCl 2be that 2:1 is made into chlorine palladium acid sodium solution with mol ratio;
(2) alumina supporter is joined in chlorine palladium acid sodium steeping fluid, steeping fluid is put into ultrasonic oscillation instrument and carry out ultrasonic oscillation dipping;
(3) ultrasonic oscillation dipping 2h, then by sample at room temperature ageing 10h;
(4) sample is put into loft drier, under the temperature condition of 80 DEG C, carry out drying;
(5) by dried sample in high temperature resistance furnace at 300 DEG C roasting 3h;
(6) prepare sodium formate solution to reduce to palladium catalyst, reduction temperature is 70 DEG C, and the recovery time is 3h, and the consumption of sodium formiate is 3 times of Palladium Content in Catalyst;
(7) reduced rear to reduction after palladium catalyst wash fully;
(8) catalyzer after washing is carried out drying under 80 DEG C of conditions, obtain shaping Pd/ aluminium oxide catalyst.
Result shows, the DNA vaccine of catalyzer reaches 95%.
[embodiment 2]
In accordance with the method for claim 1, described catalyzer is Pd/ aluminum oxide, adopts the method preparation comprised the steps:
(1) by NaCl and PdCl 2be that 2:1 is made into chlorine palladium acid sodium solution with mol ratio;
(2) alumina supporter is joined in chlorine palladium acid sodium steeping fluid, steeping fluid is put into ultrasonic oscillation instrument and carry out ultrasonic oscillation dipping;
(3) ultrasonic oscillation dipping 8h, then by sample at room temperature ageing 9h;
(4) sample is put into loft drier, under the temperature condition of 100 DEG C, carry out drying;
(5) by dried sample in high temperature resistance furnace at 600 DEG C roasting 2h;
(6) prepare sodium formate solution to reduce to palladium catalyst, reduction temperature is 100 DEG C, and the recovery time is 2h, and the consumption of sodium formiate is 6 times of Palladium Content in Catalyst;
(7) reduced rear to reduction after palladium catalyst wash fully;
(8) catalyzer after washing is carried out drying under 100 DEG C of conditions, obtain shaping Pd/ aluminium oxide catalyst.
Result shows, the DNA vaccine of catalyzer reaches 93%.
[embodiment 3]
In accordance with the method for claim 1, described catalyzer is Pd/ aluminum oxide, adopts the method preparation comprised the steps:
(1) by NaCl and PdCl 2be that 3:1 is made into chlorine palladium acid sodium solution with mol ratio;
(2) alumina supporter is joined in chlorine palladium acid sodium steeping fluid, steeping fluid is put into ultrasonic oscillation instrument and carry out ultrasonic oscillation dipping;
(3) ultrasonic oscillation dipping 5h, then by sample at room temperature ageing 12h;
(4) sample is put into loft drier, under the temperature condition of 100 DEG C, carry out drying;
(5) by dried sample in high temperature resistance furnace at 500 DEG C roasting 5h;
(6) prepare sodium formate solution to reduce to palladium catalyst, reduction temperature is 90 DEG C, and the recovery time is 5h, and the consumption of sodium formiate is 4 times of Palladium Content in Catalyst;
(7) reduced rear to reduction after palladium catalyst wash fully;
(8) catalyzer after washing is carried out drying under 100 DEG C of conditions, obtain shaping Pd/ aluminium oxide catalyst.
Result shows, the DNA vaccine of catalyzer reaches 96%.
Obviously, method of the present invention can remove the oxygen in peroxide passivation production propylene oxide tail gas, adopts the oxygen concentration in effective catalyst reduction gas mixture, the inside oxygen level of propylene surge tank in technique is not exceeded standard, do not form the system of firing, the safety of effective guarantee device reaction system; Decrease simultaneously the consumption of nitrogen and oxygen too high time propylene row torch a large amount of wastes, improve economic benefit.

Claims (5)

1. one kind removes the method for hydrogen peroxide legal system propylene oxide process gas mixture micro amount of oxygen, produce between the circulation propylene compressor of propylene oxide full scale plant and propylene surge tank at peroxide passivation and deoxidation reactor is set, the technique gas mixture of described full scale plant and hydrogen enter deoxidation reactor after gas mixer mixing, with catalyst exposure, deoxidation reactor outlet material enters propylene surge tank; Technique gas mixture pipeline before entering gas mixer arranges oxygen content analyser, and forms three with the feed valve on hydrogen pipeline and get two interlocked control, control the aperture of hydrogen feed valve; Establish oxygen content analyser at deoxidation reactor top, and form three with the control valve put on scare line at deoxidation reactor top and get two interlocked control, start interlocking when oxygen volume content is more than 5%, deoxidation reactor top gas mixture is disposed to torch; Propylene surge tank arranges oxygen content analyser, and forms three with the control valve put on scare line on propylene surge tank and get two interlocked control, start interlocking when oxygen volume content is more than 5%, the gas mixture of propylene surge tank is disposed to torch; Wherein, described catalyzer is Pd/ aluminum oxide, adopts the method preparation comprised the steps:
(1) by NaCl and PdCl 2be between 1.5 ~ 4, be made into chlorine palladium acid sodium solution with mol ratio;
(2) alumina supporter is joined in chlorine palladium acid sodium steeping fluid, steeping fluid is put into ultrasonic oscillation instrument and carry out ultrasonic oscillation dipping;
(3) ultrasonic oscillation dipping 2 ~ 8h, then by sample at room temperature ageing >=8h;
(4) sample is put into loft drier, under the temperature condition of >=80 DEG C, carry out drying;
(5) by dried sample in high temperature resistance furnace at 300 ~ 600 DEG C roasting >=2h;
(6) prepare sodium formate solution to reduce to palladium catalyst, reduction temperature is 70 ~ 100 DEG C, and the recovery time is >=2h, and the consumption of sodium formiate is 3 ~ 6 times of Palladium Content in Catalyst;
(7) reduced rear to reduction after palladium catalyst wash fully;
(8) catalyzer after washing is carried out drying under >=80 DEG C of conditions, obtain shaping Pd/ aluminium oxide catalyst.
2. a kind of method removing hydrogen peroxide legal system propylene oxide process gas mixture micro amount of oxygen according to claim 1, it is characterized in that measuring the oxygen content of deoxidation reactor import and outlet, calculate the DNA vaccine of catalyzer, the DNA vaccine of described catalyzer is greater than 90%.
3. a kind of method removing hydrogen peroxide legal system propylene oxide process gas mixture micro amount of oxygen according to claim 1, is characterized in that the reaction conditions of described deoxidation reactor is: 50 ~ 100 DEG C; 0 ~ 0.5MPa.
4. a kind of method removing hydrogen peroxide legal system propylene oxide process gas mixture micro amount of oxygen according to claim 1, is characterized in that the mass ratio of palladium and alumina supporter in described catalyzer is 1 ‰ ~ 5 ‰.
5. a kind of method removing hydrogen peroxide legal system propylene oxide process gas mixture micro amount of oxygen according to claim 1, it is characterized in that when the oxygen volume content at deoxidation reactor top is more than 1% alarm, after reporting to the police, operator need check hydrogen inlet, temperature of reaction and the residence time, and the activity of sampling and testing catalyzer.
CN201510496036.8A 2015-08-13 2015-08-13 The method for removing hydrogen peroxide legal system propylene oxide process gaseous mixture micro amount of oxygen Active CN105130928B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109748888A (en) * 2017-11-08 2019-05-14 中国石油化工股份有限公司 The method for removing the oxygen in HPPO process cycles gas
WO2019175700A1 (en) * 2018-03-13 2019-09-19 Sabic Global Technologies B.V. Photochemical deoxygenation systems and methods for the storage of liquid that generates peroxide
CN110389602A (en) * 2018-04-19 2019-10-29 中国石油化工股份有限公司 Method for controlling the content of specific gas in target container
CN113856407A (en) * 2021-10-28 2021-12-31 山东新龙集团有限公司 Method for treating tail gas in process of preparing epoxy chloropropane by oxidation method

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4943650A (en) * 1989-01-30 1990-07-24 The Boc Group, Inc. Process for the production of nitriles
US20070004926A1 (en) * 2005-06-29 2007-01-04 Basf Aktiengesellschaft Process for producing propylene oxide
EP2430009B1 (en) * 2009-05-12 2013-08-28 Basf Se Process for producing propylene oxide
CN102103368A (en) * 2010-10-27 2011-06-22 中国石油化工股份有限公司 Method for monitoring and controlling reactor oxygen concentration in epichlorohydrin production process

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109748888A (en) * 2017-11-08 2019-05-14 中国石油化工股份有限公司 The method for removing the oxygen in HPPO process cycles gas
WO2019175700A1 (en) * 2018-03-13 2019-09-19 Sabic Global Technologies B.V. Photochemical deoxygenation systems and methods for the storage of liquid that generates peroxide
CN110389602A (en) * 2018-04-19 2019-10-29 中国石油化工股份有限公司 Method for controlling the content of specific gas in target container
CN110389602B (en) * 2018-04-19 2022-09-23 中国石油化工股份有限公司 Method for controlling content of specific gas in target container
CN113856407A (en) * 2021-10-28 2021-12-31 山东新龙集团有限公司 Method for treating tail gas in process of preparing epoxy chloropropane by oxidation method

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