CN110128314A - A kind of method of bis- (tert-butyl peroxide) butane of continuous production 2,2- - Google Patents
A kind of method of bis- (tert-butyl peroxide) butane of continuous production 2,2- Download PDFInfo
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- CN110128314A CN110128314A CN201910507684.7A CN201910507684A CN110128314A CN 110128314 A CN110128314 A CN 110128314A CN 201910507684 A CN201910507684 A CN 201910507684A CN 110128314 A CN110128314 A CN 110128314A
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- butane
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- butyl peroxide
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- 239000001273 butane Substances 0.000 title claims abstract description 47
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 title claims abstract description 47
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 title claims abstract description 47
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000010924 continuous production Methods 0.000 title claims abstract description 22
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims abstract description 78
- 238000006243 chemical reaction Methods 0.000 claims abstract description 73
- 238000001816 cooling Methods 0.000 claims abstract description 51
- DKGAVHZHDRPRBM-UHFFFAOYSA-N tert-butyl alcohol Substances CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims abstract description 32
- -1 tertbutanol peroxide Chemical class 0.000 claims abstract description 30
- 239000003054 catalyst Substances 0.000 claims abstract description 29
- 230000002378 acidificating effect Effects 0.000 claims abstract description 28
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 239000003513 alkali Substances 0.000 claims abstract description 9
- 238000004140 cleaning Methods 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 239000012074 organic phase Substances 0.000 claims abstract description 9
- 238000000926 separation method Methods 0.000 claims abstract description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 76
- 239000002904 solvent Substances 0.000 claims description 27
- 239000002671 adjuvant Substances 0.000 claims description 16
- 238000006555 catalytic reaction Methods 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 14
- DKNJHLHLMWHWOI-UHFFFAOYSA-L ruthenium(2+);sulfate Chemical compound [Ru+2].[O-]S([O-])(=O)=O DKNJHLHLMWHWOI-UHFFFAOYSA-L 0.000 claims description 12
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 10
- 229960001484 edetic acid Drugs 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 2
- HVBSAKJJOYLTQU-UHFFFAOYSA-N 4-aminobenzenesulfonic acid Chemical compound NC1=CC=C(S(O)(=O)=O)C=C1 HVBSAKJJOYLTQU-UHFFFAOYSA-N 0.000 claims 1
- 229950000244 sulfanilic acid Drugs 0.000 claims 1
- 239000003208 petroleum Substances 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000003921 oil Substances 0.000 description 6
- 238000006116 polymerization reaction Methods 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 239000003431 cross linking reagent Substances 0.000 description 4
- 150000002978 peroxides Chemical class 0.000 description 4
- 230000035484 reaction time Effects 0.000 description 4
- 239000002585 base Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 3
- 150000001451 organic peroxides Chemical class 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- KWOLFJPFCHCOCG-UHFFFAOYSA-N Acetophenone Chemical compound CC(=O)C1=CC=CC=C1 KWOLFJPFCHCOCG-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 2
- 239000012847 fine chemical Substances 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 229920006305 unsaturated polyester Polymers 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000003377 acid catalyst Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 description 1
- 229940092714 benzenesulfonic acid Drugs 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 125000000864 peroxy group Chemical group O(O*)* 0.000 description 1
- 239000003505 polymerization initiator Substances 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C407/00—Preparation of peroxy compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of continuous production 2, the method for bis- (tert-butyl peroxide) butane of 2-, using following steps: (1) configuring acidic catalyst；(2) acidic catalyst, tertbutanol peroxide enter in the same pre-cooling module of microreactor and mix, and methyl ethyl ketone enters another pre-cooling module of microreactor, control the precooling temperatures of two pre-cooling modules；Enter reaction module after the pre-cooled module pre-cooling of (3) three kinds of raw materials to be reacted, reaction temperature and pre-cooling module temperature are consistent；(4) after the reaction was completed, the reaction solution exported from micro passage reaction is directly collected, liquid separation, organic phase alkali cleaning, washes, obtains the petroleum spirit of bis- (tert-butyl peroxide) butane of 2,2-.The present invention is compared with traditional still reaction, and heat exchange efficiency is high, and system heat exchanging is uniform, and reaction temperature is accurately controlled using external heat exchanger, can open at any time, stop reacting, and no enlarge-effect is highly-safe, is suitble to industrialized production.
Description
Technical field
The invention belongs to Field of Fine Chemicals more particularly to a kind of continuous production 2, bis- (tert-butyl peroxide) butane of 2-
Method.
Background technique
Organic peroxide crosslinking agent is a kind of important auxiliary agent of organic high molecular polymer, it can will be linear or slight
The organic polymer chain of branched chain type is converted to tridimensional network to limit between macromolecular chain and macromolecular chain interior chain
Between relative motion, so as to improve certain performances of organic high molecular polymer, some high molecular polymerizations by crosslinking after can
Significantly improve heat resistance, the performances such as oil resistivity, wearability, mechanical strength；Also some organic high molecular polymers, such as rubber, must
Must can just there be actual use to be worth by crosslinking.
We are cumyl peroxides usually using organic peroxide crosslinking agent, but are using this peroxide
Crosslinking agent generates the acetophenone with bad smell when crosslinking, and stays in manufactured goods, therefore this organic peroxide is handed over
Connection agent cannot use in many cases.
2,2- bis- (tert-butyl peroxide) butane be widely used in as substitute unsaturated polyester (UP) and silicon rubber crosslinking agent,
The polymerization initiator of monomer, polypropylene modifier, vulcanizer, also can be used as not machine synthesis material, be also applied to paint store
Industry is a kind of common fine chemicals.
As the initiator of polymerization reaction, being mainly used for the copolymer of suspension method styrene and styrene in temperature is 90-
Polymerization reaction within the scope of 130 DEG C.Compared with thermal-initiated polymerization, the initiation polymerization of 2,2- bis- (tert-butyl peroxide) butane has
Single residual level is low, high conversion rate, the high advantage of reaction rate.
What 2,2- bis- (tert-butyl peroxide) butane were mainly synthesized under the catalysis of acid with tertbutanol peroxide and methyl ethyl ketone.
But since this acid catalyzed process does not use solvent, play easily occurs for the peroxy ketal product and a large amount of acid catalyst of high-content
Strong sour decomposition reaction, causes product yield low, and color is deep, or even causes an explosion accident because highly exothermic, produces dangerous.
And industrial production is still produced using traditional batch process, the processing time such as charging, discharging is long, and reaction kettle volume is huge
Greatly, it needs to occupy biggish workshop, which is exothermic reaction, needs lower temperature, heat is not easy to shed, and traditional
Still reaction, mass-and heat-transfer efficiency is lower, is easy to happen safety accident.So far, there is not yet producing 2,2- in a continuous manner
The research of bis- (tert-butyl peroxide) butane.
Summary of the invention
The present invention provides a kind of continuous production 2, the method for bis- (tert-butyl peroxide) butane of 2-, using following steps:
(1) acidic catalyst is configured；
(2) acidic catalyst, tertbutanol peroxide are passed through into the same pre-cooling module that metering pump enters microreactor respectively
Middle mixing, at the same by methyl ethyl ketone by metering pump enter microreactor another pre-cooling module, control two pre-cooling modules
Precooling temperature；
Enter reaction module after the pre-cooled module pre-cooling of (3) three kinds of raw materials to be reacted, reaction temperature and pre-cooling module temperature are protected
It holds consistent；
(4) after the reaction was completed, the reaction solution exported from micro passage reaction is flowed directly into the collector equipped with solvent naphtha
In, after reaction solution stops outflow, liquid separation, organic phase alkali cleaning washes, obtains the solvent of bis- (tert-butyl peroxide) butane of 2,2-
Oil solution.
Further, in the step (2), the acidic catalyst, tertbutanol peroxide are mixed in pre-cooling module
Afterwards, catalysis adjuvant is added into pre-cooling module, the catalysis adjuvant is the mixture of ruthenium sulfate and ethylenediamine tetra-acetic acid, ruthenium sulfate
With the mixing mass ratio ruthenium sulfate of ethylenediamine tetra-acetic acid: ethylenediamine tetra-acetic acid=1:2~5；The quality of the catalysis adjuvant is described
The 10%~16% of acidic catalyst quality.
Further, the acidic catalyst be hydrochloric acid, sulfuric acid, phosphoric acid, perchloric acid, nitric acid, p-methyl benzenesulfonic acid, to ammonia
The mixing of one or more of base benzene sulfonic acid.
Further, the acidic catalyst is sulfuric acid.
Further, Solute mass percentage composition is 45%-95% in the acidic catalyst, and solvent is water.
Further, Solute mass percentage composition is 60%-80% in the acidic catalyst, and solvent is water.
Further, in reaction module, mole of solute, methyl ethyl ketone and tertbutanol peroxide in the acidic catalyst
Than the solute in acidic catalyst: methyl ethyl ketone: tertbutanol peroxide=0.4~1.2:1:2.
Further, the precooling temperature and reaction temperature are 6 DEG C~15 DEG C.
As can be seen from the above technical solutions, the invention has the advantages that
1, the present invention provides a kind of is existed in a manner of continuous flow using tertbutanol peroxide and methyl ethyl ketone in micro passage reaction
It is catalyzed lower continuous production 2, the process route of bis- (tert-butyl peroxide) butane of 2-.The process route advantage is accurately to control
Reaction temperature, mole residence time etc. when reacted of raw material, higher yields obtains in tens seconds to a few minutes clock time
2,2- bis- (tert-butyl peroxide) butane.This is that the production of bis- (tert-butyl peroxide) butane of 2,2- provides one easily to operate
Safe synthetic route.And the present invention is using the method continuous production 2 continuously prepared in micro passage reaction, bis- (the peroxidating uncles of 2-
Butyl) butane, it is compared with tradition still reaction, heat exchange efficiency is high, and system heat exchanging is uniform, and reaction temperature can using external heat exchanger
Accurate control, can open at any time, stop reacting, and no enlarge-effect is highly-safe, be suitble to industrialized production.
2, the present invention further increases catalysis effect by introducing catalysis adjuvant under acidic catalyst catalyst system
Power, the purity of 2,2- bis- (tert-butyl peroxide) butane products have wide compared with significantly improving in the case where without catalysis adjuvant
Application prospect.
Detailed description of the invention
Fig. 1 is the flow diagram of the method for the invention；Wherein raw material 1 represents acidic catalyst；Raw material 2 represents peroxide
Change the tert-butyl alcohol；Raw material 3 represents methyl ethyl ketone.
Specific embodiment
It is described in detail below with reference to embodiment:
Embodiment 1
A kind of continuous production 2, the method for bis- (tert-butyl peroxide) butane of 2- comprising the steps of:
(1) sulfuric acid that configuration Solute mass fraction is 60%, solvent is water；
(2) sulfuric acid of configuration, tertbutanol peroxide are passed through into metering pump respectively enter in the same pre-cooling module of microreactor and mix
It closes, while methyl ethyl ketone being entered to another pre-cooling module of microreactor by metering pump, control the pre- of two pre-cooling modules
Cold temperature is 15 DEG C；
Enter reaction module after the pre-cooled module pre-cooling of (3) three kinds of raw materials to be reacted, adjusts the flow velocity of metering pump, make to react mould
The molar ratio sulfuric acid (solute in sulfuric acid solution) of sulfuric acid, methyl ethyl ketone and tertbutanol peroxide in block: methyl ethyl ketone: the tertiary fourth of peroxidating
Alcohol=0.8:1:2, reaction time are 150 seconds；Reaction temperature and pre-cooling module temperature are consistent；
(4) after the reaction was completed, the reaction solution exported from micro passage reaction is flowed directly into the collector equipped with solvent naphtha
In, after reaction solution stops outflow, liquid separation, organic phase alkali cleaning washes, obtains the solvent of bis- (tert-butyl peroxide) butane of 2,2-
Oil solution.Product 2 in petroleum spirit is measured, the purity of bis- (tert-butyl peroxide) butane of 2- is 93.02%.
Embodiment 2
A kind of continuous production 2, the method for bis- (tert-butyl peroxide) butane of 2- comprising the steps of:
(1) sulfuric acid that configuration Solute mass fraction is 70%, solvent is water；
(2) sulfuric acid of configuration, tertbutanol peroxide are passed through into metering pump respectively enter in the same pre-cooling module of microreactor and mix
It closes, while methyl ethyl ketone being entered to another pre-cooling module of microreactor by metering pump, control the pre- of two pre-cooling modules
Cold temperature is 8 DEG C；
Enter reaction module after the pre-cooled module pre-cooling of (3) three kinds of raw materials to be reacted, adjusts the flow velocity of metering pump, make to react mould
The molar ratio sulfuric acid (solute in sulfuric acid solution) of sulfuric acid, methyl ethyl ketone and tertbutanol peroxide in block: methyl ethyl ketone: the tertiary fourth of peroxidating
Alcohol=0.6:1:2, reaction time are 200 seconds；Reaction temperature and pre-cooling module temperature are consistent；
(4) after the reaction was completed, the reaction solution exported from micro passage reaction is flowed directly into the collector equipped with solvent naphtha
In, after reaction solution stops outflow, liquid separation, organic phase alkali cleaning washes, obtains the solvent of bis- (tert-butyl peroxide) butane of 2,2-
Oil solution.Product 2 in petroleum spirit is measured, the purity of bis- (tert-butyl peroxide) butane of 2- is 92.42%.
Embodiment 3
A kind of continuous production 2, the method for bis- (tert-butyl peroxide) butane of 2- comprising the steps of:
(1) sulfuric acid that configuration Solute mass fraction is 75%, solvent is water；
(2) sulfuric acid of configuration, tertbutanol peroxide are passed through into metering pump respectively enter in the same pre-cooling module of microreactor and mix
It closes, while methyl ethyl ketone being entered to another pre-cooling module of microreactor by metering pump, control the pre- of two pre-cooling modules
Cold temperature is 6 DEG C；
Enter reaction module after the pre-cooled module pre-cooling of (3) three kinds of raw materials to be reacted, adjusts the flow velocity of metering pump, make to react mould
The molar ratio sulfuric acid (solute in sulfuric acid solution) of sulfuric acid, methyl ethyl ketone and tertbutanol peroxide in block: methyl ethyl ketone: the tertiary fourth of peroxidating
Alcohol=0.75:1:2, reaction time are 100 seconds；Reaction temperature and pre-cooling module temperature are consistent；
(4) after the reaction was completed, the reaction solution exported from micro passage reaction is flowed directly into the collector equipped with solvent naphtha
In, after reaction solution stops outflow, liquid separation, organic phase alkali cleaning washes, obtains the solvent of bis- (tert-butyl peroxide) butane of 2,2-
Oil solution.Product 2 in petroleum spirit is measured, the purity of bis- (tert-butyl peroxide) butane of 2- is 92.35%.
Embodiment 4
A kind of continuous production 2, the method for bis- (tert-butyl peroxide) butane of 2- comprising the steps of:
(1) sulfuric acid that configuration Solute mass fraction is 80%, solvent is water；
(2) sulfuric acid of configuration, tertbutanol peroxide are passed through into metering pump respectively enter in the same pre-cooling module of microreactor and mix
It closes, while methyl ethyl ketone being entered to another pre-cooling module of microreactor by metering pump, control the pre- of two pre-cooling modules
Cold temperature is 10 DEG C；
Enter reaction module after the pre-cooled module pre-cooling of (3) three kinds of raw materials to be reacted, adjusts the flow velocity of metering pump, make to react mould
The molar ratio sulfuric acid (solute in sulfuric acid solution) of sulfuric acid, methyl ethyl ketone and tertbutanol peroxide in block: methyl ethyl ketone: the tertiary fourth of peroxidating
Alcohol=0.7:1:2, reaction time are 85 seconds；Reaction temperature and pre-cooling module temperature are consistent；
(4) after the reaction was completed, the reaction solution exported from micro passage reaction is flowed directly into the collector equipped with solvent naphtha
In, after reaction solution stops outflow, liquid separation, organic phase alkali cleaning washes, obtains the solvent of bis- (tert-butyl peroxide) butane of 2,2-
Oil solution.Product 2 in petroleum spirit is measured, the purity of bis- (tert-butyl peroxide) butane of 2- is 93.03%.
Comparative example 1
A kind of continuous production 2, the method for bis- (tert-butyl peroxide) butane of 2- comprising the steps of:
(1) sulfuric acid that configuration Solute mass fraction is 80%, solvent is water；
(2) sulfuric acid of configuration, tertbutanol peroxide are passed through into metering pump respectively enter in the same pre-cooling module of microreactor and mix
It closes, while methyl ethyl ketone being entered to another pre-cooling module of microreactor by metering pump, control the pre- of two pre-cooling modules
Cold temperature is 10 DEG C, while being pumped into sulfuric acid, tertbutanol peroxide, to sulfuric acid, the pre-cooling module of tertbutanol peroxide mixing
In be continuously added to catalysis adjuvant, catalysis adjuvant is the mixture of ruthenium sulfate and ethylenediamine tetra-acetic acid, ruthenium sulfate and ethylenediamine tetrem
The mixing mass ratio ruthenium sulfate of acid: ethylenediamine tetra-acetic acid=1:5；The addition of control catalysis adjuvant, so that being catalyzed in reaction module auxiliary
The quality of agent is 16% of acidic catalyst quality (solute+solvent) in reaction module；
(3) enter reaction module after the pre-cooled module pre-cooling of raw material to be reacted, adjust the flow velocity of metering pump, make sulfuric acid, first and second
The molar ratio sulfuric acid (solute in sulfuric acid solution) of ketone and tertbutanol peroxide: methyl ethyl ketone: tertbutanol peroxide=0.7:1:2, instead
Answering the residence time is 85 seconds；Reaction temperature and pre-cooling module temperature are consistent；
(4) after the reaction was completed, the reaction solution exported from micro passage reaction is flowed directly into the collector equipped with solvent naphtha
In, after reaction solution stops outflow, liquid separation, organic phase alkali cleaning, washing, which removes, is catalyzed adjuvant, obtains bis- (the tertiary fourths of peroxidating of 2,2-
Base) butane petroleum spirit.Product 2 in petroleum spirit is measured, the purity of bis- (tert-butyl peroxide) butane of 2- is
97.57%。
Comparative example 2
A kind of continuous production 2, the method for bis- (tert-butyl peroxide) butane of 2- comprising the steps of:
(1) sulfuric acid that configuration Solute mass fraction is 80%, solvent is water；
(2) sulfuric acid of configuration, tertbutanol peroxide are passed through into metering pump respectively enter in the same pre-cooling module of microreactor and mix
It closes, while methyl ethyl ketone being entered to another pre-cooling module of microreactor by metering pump, control the pre- of two pre-cooling modules
Cold temperature is 10 DEG C, while being pumped into sulfuric acid, tertbutanol peroxide, to sulfuric acid, the pre-cooling module of tertbutanol peroxide mixing
In be continuously added to catalysis adjuvant, catalysis adjuvant is the mixture of ruthenium sulfate and ethylenediamine tetra-acetic acid, ruthenium sulfate and ethylenediamine tetrem
The mixing mass ratio ruthenium sulfate of acid: ethylenediamine tetra-acetic acid=1:2；The addition of control catalysis adjuvant, so that being catalyzed in reaction module auxiliary
The quality of agent is 10% of acidic catalyst quality (solute+solvent) in reaction module；
(3) enter reaction module after the pre-cooled module pre-cooling of raw material to be reacted, adjust the flow velocity of metering pump, make sulfuric acid, first and second
The molar ratio sulfuric acid (solute in sulfuric acid solution) of ketone and tertbutanol peroxide: methyl ethyl ketone: tertbutanol peroxide=0.7:1:2, instead
Answering the residence time is 85 seconds；Reaction temperature and pre-cooling module temperature are consistent；
(4) after the reaction was completed, the reaction solution exported from micro passage reaction is flowed directly into the collector equipped with solvent naphtha
In, after reaction solution stops outflow, liquid separation, organic phase alkali cleaning, washing, which removes, is catalyzed adjuvant, obtains bis- (the tertiary fourths of peroxidating of 2,2-
Base) butane petroleum spirit.Product 2 in petroleum spirit is measured, the purity of bis- (tert-butyl peroxide) butane of 2- is
96.42%。
Comparative example 3~8
6 mutual independent tests are carried out respectively, and test is according to continuous production 2 as described in example 4, the bis- (peroxides of 2- every time
Change tert-butyl) method of butane prepares the petroleum spirit of bis- (tert-butyl peroxide) butane of 2,2-, and difference is only in that:
Test acidic catalyst type used is different every time, and other technological parameters are identical with embodiment 4.Each embodiment institute
Mass percentage with acidic catalyst and its solute is as shown in table 1.2,2- obtained by each embodiment is bis- (tert-butyl peroxide)
The petroleum spirit of butane measures product 2, and the purity of bis- (tert-butyl peroxide) butane of 2-, the results are shown in Table 1.
。
Technical solution provided by the present invention is described in detail above, for those of ordinary skill in the art,
Thought according to an embodiment of the present invention, there will be changes in the specific implementation manner and application range, in conclusion this theory
Bright book content should not be construed as limiting the invention.
Claims (8)
1. a kind of continuous production 2, the method for bis- (tert-butyl peroxide) butane of 2-, which is characterized in that use following steps:
(1) acidic catalyst is configured；
(2) acidic catalyst, tertbutanol peroxide are passed through into the same pre-cooling module that metering pump enters microreactor respectively
Middle mixing, at the same by methyl ethyl ketone by metering pump enter microreactor another pre-cooling module, control two pre-cooling modules
Precooling temperature；
Enter reaction module after the pre-cooled module pre-cooling of (3) three kinds of raw materials to be reacted, reaction temperature and pre-cooling module temperature are protected
It holds consistent；
(4) after the reaction was completed, the reaction solution exported from micro passage reaction is flowed directly into the collector equipped with solvent naphtha
In, after reaction solution stops outflow, liquid separation, organic phase alkali cleaning washes, obtains the solvent of bis- (tert-butyl peroxide) butane of 2,2-
Oil solution.
2. a kind of continuous production 2 according to claim 1, the method for bis- (tert-butyl peroxide) butane of 2-, feature exist
In in the step (2), after the acidic catalyst, tertbutanol peroxide are mixed in pre-cooling module, into pre-cooling module
Catalysis adjuvant is added, the catalysis adjuvant is the mixture of ruthenium sulfate and ethylenediamine tetra-acetic acid, ruthenium sulfate and ethylenediamine tetra-acetic acid
Mixing mass ratio ruthenium sulfate: ethylenediamine tetra-acetic acid=1:2~5；The quality of the catalysis adjuvant is the acidic catalyst quality
10%~16%.
3. a kind of continuous production 2 according to claim 1 or 2, the method for bis- (tert-butyl peroxide) butane of 2-, feature
Be, the acidic catalyst is hydrochloric acid, sulfuric acid, phosphoric acid, perchloric acid, nitric acid, p-methyl benzenesulfonic acid, in p-aminobenzene sulfonic acid
One or more of mixing.
4. a kind of continuous production 2 according to claim 3, the method for bis- (tert-butyl peroxide) butane of 2-, feature exist
In the acidic catalyst is sulfuric acid.
5. a kind of continuous production 2 according to claim 1 or 2, the method for bis- (tert-butyl peroxide) butane of 2-, feature
It is, Solute mass percentage composition is 45%-95% in the acidic catalyst, and solvent is water.
6. a kind of continuous production 2 according to claim 5, the method for bis- (tert-butyl peroxide) butane of 2-, feature exist
In Solute mass percentage composition is 60%-80% in the acidic catalyst, and solvent is water.
7. a kind of continuous production 2 according to claim 1 or 2, the method for bis- (tert-butyl peroxide) butane of 2-, feature
It is, in reaction module, the molar ratio acidic catalyst of solute, methyl ethyl ketone and tertbutanol peroxide in the acidic catalyst
In solute: methyl ethyl ketone: tertbutanol peroxide=0.4~1.2:1:2.
8. a kind of continuous production 2 according to claim 1 or 2, the method for bis- (tert-butyl peroxide) butane of 2-, feature
It is, the precooling temperature and reaction temperature are 6 DEG C~15 DEG C.
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