CN107056670B - A kind of preparation method of two tertiary base peroxide - Google Patents
A kind of preparation method of two tertiary base peroxide Download PDFInfo
- Publication number
- CN107056670B CN107056670B CN201710442695.2A CN201710442695A CN107056670B CN 107056670 B CN107056670 B CN 107056670B CN 201710442695 A CN201710442695 A CN 201710442695A CN 107056670 B CN107056670 B CN 107056670B
- Authority
- CN
- China
- Prior art keywords
- tert
- peroxide
- micro
- butyl alcohol
- butyl
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 150000002978 peroxides Chemical class 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims abstract description 164
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 74
- 238000006243 chemical reaction Methods 0.000 claims abstract description 55
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000003054 catalyst Substances 0.000 claims abstract description 26
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 43
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 230000008859 change Effects 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 238000006555 catalytic reaction Methods 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 16
- 238000000034 method Methods 0.000 abstract description 16
- 230000008569 process Effects 0.000 abstract description 5
- 238000010924 continuous production Methods 0.000 abstract description 2
- -1 tert-butyl alcohol peroxide Chemical class 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 18
- 239000000463 material Substances 0.000 description 17
- 230000035484 reaction time Effects 0.000 description 12
- 238000000926 separation method Methods 0.000 description 10
- 238000004817 gas chromatography Methods 0.000 description 9
- 238000005406 washing Methods 0.000 description 9
- 238000004458 analytical method Methods 0.000 description 8
- 239000012043 crude product Substances 0.000 description 8
- 238000001035 drying Methods 0.000 description 8
- 229910001220 stainless steel Inorganic materials 0.000 description 8
- 239000010935 stainless steel Substances 0.000 description 8
- 239000002585 base Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- PAOHAQSLJSMLAT-UHFFFAOYSA-N 1-butylperoxybutane Chemical compound CCCCOOCCCC PAOHAQSLJSMLAT-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 239000002808 molecular sieve Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000005554 pickling Methods 0.000 description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 2
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 238000005502 peroxidation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C407/00—Preparation of peroxy compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention discloses a kind of preparation methods of two tertiary base peroxide, by the tert-butyl alcohol, hydrogen peroxide, catalyst is introduced into micro-reaction device in a continuous manner, so that peroxidization occurs for the tert-butyl alcohol and hydrogen peroxide, the logistics comprising di-tert-butyl peroxide is made, then draws the logistics comprising di-tert-butyl peroxide from micro-reaction device, it separated, washed, be dried to obtain di-tert-butyl peroxide；Wherein the tert-butyl alcohol and peroxide mole ratio are 1:2~1:2.2, and catalyst amount accounts for the tert-butyl alcohol, the 10~20% of hydrogen peroxide and catalyst gross mass.Present invention process is simple, and using the good micro-reaction device continuous production of safety, and the tert-butyl alcohol peroxide reactions selectivity prepared is high, and yield is good, reduces production process, reduces production cost.
Description
Technical field
The invention belongs to chemical industry synthesis fields, and in particular to a kind of preparation method of two tertiary base peroxide.
Background technique
O -- O bond decomposition activation energy in di-tert-butyl peroxide is very low, easily resolves into oxygen radical or oxygen-containing chemical combination
Object, the initiator of chain reaction when being diesel combustion, reduce diesel combustion reaction initial temperature, so as to improve diesel oil
Fiery performance can be used as the additive for improving diesel cetane-number.Hydroperoxidation method is industrial production t-butyl peroxy
Change the main method of hydrogen and di-tert-butyl peroxide, domestic manufacturing enterprise is all made of technique production at present.It is used
35% hydrogen peroxide is mixed with the tert-butyl alcohol, and makees catalyst with 70% concentrated sulfuric acid, after reacting a few hours, water-oil separating, and oil
30% neutralizing treatment, liquid separation are mutually used, upper layer product is di-tert-butyl peroxide, and lower layer's product pickling, liquid separation again obtains
Tert-butyl hydroperoxide.In order to control the decomposition of hydrogen peroxide in reaction process, and guarantee the safety of process, often in cryogenic freezing shape
It is carried out under state, reaction temperature is normally controlled in 5 DEG C or less.But the reaction process route is longer, uses pickling and alkali repeatedly
It washes, wastewater flow rate is bigger.Also there is the patent of a small amount of di-tert-butyl peroxide in the country, as 203530185 U of CN discloses one kind
The process units of di-tert-butyl peroxide, the device be added in original production technology link equipped with active carbon except different
Gaseous impurity in production process can be filtered out, improve the safety in production process by taste tank, be conducive to the smooth of production
It carries out.1699339 A of CN discloses a kind of method using Titanium Sieve Molecular Sieve as catalyst preparation di-tert-butyl peroxide,
The disadvantage is that the conversion ratio of the tert-butyl alcohol is lower, product yield is not high.104557652 A of CN discloses a kind of using acid ion
The method that resins as catalysts synthesizes di-tert-butyl peroxide, catalyst can be recycled, and reduce production cost, but tertiary fourth
The selectivity of base peroxidization is not high, and product is di-tert-butyl peroxide and single tert-butyl peroxide mixture, later period
Need separating technology.103204792 A of CN discloses a kind of side that soluble zinc salt makees system with molecular sieve for preparing for di-tert-butyl peroxide
Method, this method do not use any acidic catalyst, reduce the corrosion losses of equipment, but product need to carry out washing process, metal
Zn-ef ficiency impurity may have residual.
In traditional autoclave production, the tert-butyl alcohol need to obtain di-tert-butyl peroxide by two-step method, i.e., first obtain single uncle
Butylperoxide, then secondary peroxidization is carried out as raw material, the reaction mechanism is as follows:
In formula, R indicates tert-butyl.
There are charge temperature requirement harshnesses (- 5 DEG C~0 DEG C) for this method, and the reaction time is long (about 4h), and security risk height etc. lacks
Point, while there are first step intermediate list tert-butyl peroxide impurity in product, the later period needs to separate.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of two tertiary base peroxide, to overcome the above-mentioned prior art to deposit
Defect, present invention process is simple, using the good micro-reaction device continuous production of safety, and the tert-butyl alcohol peroxidating prepared
Object reaction selectivity is high, and yield is good, reduces production process, reduces production cost.
In order to achieve the above objectives, the present invention adopts the following technical scheme:
A kind of preparation method of two tertiary base peroxide, by the tert-butyl alcohol, hydrogen peroxide, catalyst introduces in a continuous manner
In micro-reaction device, so that peroxidization occurs for the tert-butyl alcohol and hydrogen peroxide, the object comprising di-tert-butyl peroxide is made
Stream, then the logistics comprising di-tert-butyl peroxide is drawn, separated, washed, be dried to obtain two from micro-reaction device
Tert-butyl peroxide；
Wherein the tert-butyl alcohol and peroxide mole ratio are 1:2~1:2.2, and catalyst amount accounts for the tert-butyl alcohol, hydrogen peroxide and
The 10~20% of catalyst gross mass.
Further, the micro-reaction device is respectively used to the conveying tert-butyl alcohol, hydrogen peroxide and catalyst including three
Micro- constant-flux pump, the outlet end of three micro- constant-flux pumps is connected to micro-mixer, and the outlet end of micro-mixer is connected to microreactor,
The outlet section of microreactor is connected with product collector.
Further, the microreactor is tubular reactor, and the internal diameter of tubular reactor is 0.5~3mm, and length is
10~30m.
Further, insulating box is provided on the outside of microreactor.
Further, the temperature of insulating box is 30~60 DEG C.
Further, it is 5~30mL/min that the tert-butyl alcohol, hydrogen peroxide and catalyst, which enter the overall flow rate of micro-reaction device,.
Further, the catalyst is the sulfuric acid that mass concentration is 98%.
Further, the temperature of peroxidization is 30~60 DEG C, and the time is 20~220s.
Compared with prior art, the invention has the following beneficial technical effects:
By the present invention in that carrying out the preparation of di-tert-butyl peroxide with micro-reaction device, there is continuity of operation, instead
Answer condition easy to control, the reaction time is short, it is highly-safe the features such as, in addition the present invention passes through the micro-tubular structure inside micro-reaction device
Feature and the strong feature of heat and mass power carry out quick peroxidization to the tert-butyl alcohol, and selectivity is strong, di-tert-butyl peroxide
Selectivity be greater than 99%, conversion ratio is greater than 99%, and the present invention can directly apply actual production, no enlarge-effect, and can basis
Needs of production is accomplished scale production.
Further, by using micro passage reaction technology, the tert-butyl alcohol only needs one-step method that can generate di-t-butyl mistake
Oxide, i.e., under the catalytic action of sulfuric acid, the tert-butyl alcohol of two molecules directly generates two tertiary fourths with a molecule peroxide reactions
Base peroxide, gas-chromatography monitor, and occur in reaction process without single tert-butyl peroxide, and product is not necessarily to secondary refining, instead
Answer mechanism as follows:
In formula, R indicates tert-butyl；After improvement, feeding temperature be can be improved to 30 DEG C or more, the reaction time shorten to 4min with
It is interior, energy consumption is thus greatly reduced, the economic benefit of production process is improved, while reducing security risk.
Detailed description of the invention
Fig. 1 is the process flow diagram that micro-reaction device synthesizes di-tert-butyl peroxide, and wherein A1, A2, A3 distinguish
For first, second, third micro- constant-flux pump, B is micro-mixer, and C is microreactor, D is insulating box, E is product collector, and R1 is
The tert-butyl alcohol, R2 are hydrogen peroxide, and R3 is sulfuric acid.
Specific embodiment
Embodiments of the present invention are described in further detail below:
A kind of preparation method of two tertiary base peroxide, by the tert-butyl alcohol, hydrogen peroxide, catalyst introduces in a continuous manner
In micro-reaction device, the overall flow rate that the tert-butyl alcohol, hydrogen peroxide and catalyst enter micro-reaction device is 5~30mL/min, i.e. uncle
It is 5~30mL/min that butanol, hydrogen peroxide and catalyst, which obtain the sum of flow velocity, so that peroxidation occurs for the tert-butyl alcohol and hydrogen peroxide
It answers, reaction temperature is 30~60 DEG C, and the time is 26~218s, and the logistics comprising di-tert-butyl peroxide is made, then will packet
Logistics containing di-tert-butyl peroxide is drawn from micro-reaction device, is separated, is washed, is dried to obtain di-tert-butyl peroxide
Object, wherein catalyst is the sulfuric acid that mass concentration is 98%；
Wherein the tert-butyl alcohol and peroxide mole ratio are 1:2~1:2.2, and catalyst amount accounts for the tert-butyl alcohol, hydrogen peroxide and
The 10~20% of catalyst gross mass；The micro-reaction device include three be respectively used to conveying the tert-butyl alcohol, hydrogen peroxide and
Micro- constant-flux pump of catalyst, the outlet end of three micro- constant-flux pumps are connected to micro-mixer, and the outlet end of micro-mixer is connected to micro-
The outlet section of reactor, microreactor is connected with product collector；Microreactor is tubular reactor, the internal diameter of tubular reactor
For 0.5~3mm, length is 10~20m, its main feature is that internal easily form turbulent flow, material good mixing effect, and heating surface area is big,
Heat transfer rate is fast, and the reaction time is abundant, and microreactor can realize that quantity is amplified, and produces on demand, no enlarge-effect；Microreactor
Outside is provided with insulating box.
Below with reference to embodiment, the invention will be described in further detail:
Embodiment 1
As shown in Figure 1, by the tert-butyl alcohol, hydrogen peroxide, sulfuric acid respectively by first micro- constant-flux pump A1, second micro- constant-flux pump A2,
The micro- constant-flux pump A3 of third is conveyed into micro-mixer B (T-type Stainless steel tee, internal diameter 0.5mm), uniform hybrid reaction, and charging is total
Rate is 5mL/min, and the molar ratio of the tert-butyl alcohol and hydrogen peroxide is 1:2, and sulfuric acid dosage is the 10% of whole quality of material.It is micro- anti-
Answering device C length is 10m, is placed in insulating box D (30 DEG C), reaction time 26s.Material is sufficiently anti-in microreactor
Product collector E should be entered afterwards.Crude product is after separation, washing, drying, gas chromatography analysis peroxide component, two uncles
Butylperoxide content is 89.7%, and single tert-butyl peroxide content is 10.2%.Tert-butyl alcohol conversion ratio 98.1%.
Embodiment 2
As shown in Figure 1, by the tert-butyl alcohol, hydrogen peroxide, sulfuric acid respectively by first micro- constant-flux pump A1, second micro- constant-flux pump A2,
The micro- constant-flux pump A3 of third is conveyed into micro-mixer B (T-type Stainless steel tee, internal diameter 0.5mm), uniform hybrid reaction, and charging is total
Rate is 5mL/min, and the molar ratio of the tert-butyl alcohol and hydrogen peroxide is 1:2.02, and sulfuric acid dosage is the 10% of whole quality of material.
Microreactor C length is 10m, is placed in insulating box D (30 DEG C), reaction time 26s.Material fills in microreactor
Enter product collector E after dividing reaction.Crude product is after separation, washing, drying, gas chromatography analysis peroxide component,
Di-tert-butyl peroxide content is 91.6%, and single tert-butyl peroxide content is 8.2%.Tert-butyl alcohol conversion ratio 99.3%.
Embodiment 3
As shown in Figure 1, by the tert-butyl alcohol, hydrogen peroxide, sulfuric acid respectively by first micro- constant-flux pump A1, second micro- constant-flux pump A2,
The micro- constant-flux pump A3 of third is conveyed into micro-mixer B (T-type Stainless steel tee, internal diameter 1mm), uniform hybrid reaction, feeds total speed
Rate is 10mL/min, and the molar ratio of the tert-butyl alcohol and hydrogen peroxide is 1:2.05, and sulfuric acid dosage is the 15% of whole quality of material.It is micro-
Reactor C length is 10m, is placed in insulating box D (40 DEG C), reaction time 51s.Material is abundant in microreactor
Enter product receiving flask E after reaction.Crude product is after separation, washing, drying, gas chromatography analysis peroxide component, and two
Tert-butyl peroxide content is 93.7%, and single tert-butyl peroxide content is 5.9%.Tert-butyl alcohol conversion ratio 99.4%.
Embodiment 4
As shown in Figure 1, by the tert-butyl alcohol, hydrogen peroxide, sulfuric acid respectively by first micro- constant-flux pump A1, second micro- constant-flux pump A2,
The micro- constant-flux pump A3 of third is conveyed into micro-mixer B (T-type Stainless steel tee, internal diameter 1mm), uniform hybrid reaction, feeds total speed
Rate is 12mL/min, and the molar ratio of the tert-butyl alcohol and hydrogen peroxide is 1:2.1, and sulfuric acid dosage is the 15% of whole quality of material.It is micro-
Reactor C length is 15m, is placed in insulating box D (45 DEG C), reaction time 51s.Material is abundant in microreactor
Enter product collector E after reaction.Crude product is after separation, washing, drying, gas chromatography analysis peroxide component, and two
Tert-butyl peroxide content is 93.5%, and single tert-butyl peroxide content is 6.2%.Tert-butyl alcohol conversion ratio 99.4%.
Embodiment 5
As shown in Figure 1, by the tert-butyl alcohol, hydrogen peroxide, sulfuric acid respectively by first micro- constant-flux pump A1, second micro- constant-flux pump A2,
The micro- constant-flux pump A3 of third is conveyed into micro-mixer B (T-type Stainless steel tee, internal diameter 2mm), uniform hybrid reaction, feeds total speed
Rate is 20mL/min, and the molar ratio of the tert-butyl alcohol and hydrogen peroxide is 1:2.1, and sulfuric acid dosage is the 15% of whole quality of material.It is micro-
Reactor C length is 15m, is placed in insulating box D (50 DEG C), reaction time 160s.Material fills in microreactor
Enter product collector E after dividing reaction.Crude product is after separation, washing, drying, gas chromatography analysis peroxide component,
Di-tert-butyl peroxide content is 92.9%, and single tert-butyl peroxide content is 6.9%.Tert-butyl alcohol conversion ratio 99.7%.
Embodiment 6
As shown in Figure 1, by the tert-butyl alcohol, hydrogen peroxide, sulfuric acid respectively by first micro- constant-flux pump A1, second micro- constant-flux pump A2,
The micro- constant-flux pump A3 of third is conveyed into micro-mixer B (T-type Stainless steel tee, internal diameter 2mm), uniform hybrid reaction, feeds total speed
Rate is 25mL/min, and the molar ratio of the tert-butyl alcohol and hydrogen peroxide is 1:2.1, and sulfuric acid dosage is the 18% of whole quality of material.It is micro-
Reactor C length is 20m, is placed in insulating box D (50 DEG C), reaction time 162s.Material fills in microreactor
Enter product collector E after dividing reaction.Crude product is after separation, washing, drying, gas chromatography analysis peroxide component,
Di-tert-butyl peroxide content is 97.0%, and single tert-butyl peroxide content is 2.9%.Tert-butyl alcohol conversion ratio 99.5%.
Embodiment 7
As shown in Figure 1, by the tert-butyl alcohol, hydrogen peroxide, sulfuric acid respectively by first micro- constant-flux pump A1, second micro- constant-flux pump A2,
The micro- constant-flux pump A3 of third is conveyed into micro-mixer B (T-type Stainless steel tee, internal diameter 3mm), uniform hybrid reaction, feeds total speed
Rate is 30mL/min, and the molar ratio of the tert-butyl alcohol and hydrogen peroxide is 1:2.2, and sulfuric acid dosage is the 20% of whole quality of material.It is micro-
Reactor C length is 15m, is placed in insulating box D (50 DEG C), reaction time 218s.Material fills in microreactor
Enter product collector E after dividing reaction.Crude product is after separation, washing, drying, gas chromatography analysis peroxide component,
Di-tert-butyl peroxide content is 99.0%, and single tert-butyl peroxide content is 0.9%.Tert-butyl alcohol conversion ratio 99.8%.
Embodiment 8
As shown in Figure 1, by the tert-butyl alcohol, hydrogen peroxide, sulfuric acid respectively by first micro- constant-flux pump A1, second micro- constant-flux pump A2,
The micro- constant-flux pump A3 of third is conveyed into micro-mixer B (T-type Stainless steel tee, internal diameter 3mm), uniform hybrid reaction, feeds total speed
Rate is 30mL/min, and the molar ratio of the tert-butyl alcohol and hydrogen peroxide is 1:2.1, and sulfuric acid dosage is the 20% of whole quality of material.It is micro-
Reactor C length is 10m, is placed in insulating box D (60 DEG C), reaction time 151s.Material fills in microreactor
Enter product collector E after dividing reaction.Crude product is after separation, washing, drying, gas chromatography analysis peroxide component,
Di-tert-butyl peroxide content is 99.6%, and single tert-butyl peroxide content is 0.3%.Tert-butyl alcohol conversion ratio 99.8%.
Claims (5)
1. a kind of preparation method of two tertiary base peroxide, which is characterized in that by the tert-butyl alcohol, hydrogen peroxide, catalyst is with continuous
Mode be introduced into micro-reaction device so that peroxidization occurs for the tert-butyl alcohol and hydrogen peroxide, the temperature of peroxidization is
30~60 DEG C, the time is 20~220s, and the logistics comprising di-tert-butyl peroxide is made, then will include di-t-butyl peroxide
The logistics of compound is drawn from micro-reaction device, is separated, is washed, is dried to obtain di-tert-butyl peroxide；
Wherein the tert-butyl alcohol and peroxide mole ratio are 1:2~1:2.2, and catalyst amount accounts for the tert-butyl alcohol, hydrogen peroxide and catalysis
The 10~20% of agent gross mass；
The micro-reaction device includes three micro- constant-flux pumps for being respectively used to the conveying tert-butyl alcohol, hydrogen peroxide and catalyst, and three
The outlet end of a micro- constant-flux pump is connected to micro-mixer, and the outlet end of micro-mixer is connected to microreactor, and microreactor goes out
Mouth section is connected with product collector, and the microreactor is tubular reactor, and the internal diameter of tubular reactor is 0.5~3mm, long
Degree is 10~30m.
2. a kind of preparation method of two tertiary base peroxide according to claim 1, which is characterized in that outside microreactor
Side is provided with insulating box.
3. a kind of preparation method of two tertiary base peroxide according to claim 2, which is characterized in that the temperature of insulating box
It is 30~60 DEG C.
4. a kind of preparation method of two tertiary base peroxide according to claim 1, which is characterized in that the tert-butyl alcohol, peroxide
Change hydrogen and catalyst enters the overall flow rate of micro-reaction device for 5~30mL/min.
5. a kind of preparation method of two tertiary base peroxide according to claim 1, which is characterized in that the catalyst
The sulfuric acid for being 98% for mass concentration.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710442695.2A CN107056670B (en) | 2017-06-13 | 2017-06-13 | A kind of preparation method of two tertiary base peroxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710442695.2A CN107056670B (en) | 2017-06-13 | 2017-06-13 | A kind of preparation method of two tertiary base peroxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107056670A CN107056670A (en) | 2017-08-18 |
| CN107056670B true CN107056670B (en) | 2019-02-26 |
Family
ID=59594952
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710442695.2A Active CN107056670B (en) | 2017-06-13 | 2017-06-13 | A kind of preparation method of two tertiary base peroxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107056670B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109331871B (en) * | 2018-11-20 | 2021-03-26 | 淄博正华助剂股份有限公司 | Synthesis method of peroxycarboxylic acid tert-butyl/amyl ester |
| CN110204472B (en) * | 2019-06-29 | 2021-05-25 | 淄博正华助剂股份有限公司 | Synthesis method of di-tert-butyl peroxide |
| CN115124446B (en) * | 2022-07-05 | 2024-01-26 | 常熟市滨江化工有限公司 | Purification method of di-tert-butyl peroxide |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102005049294C5 (en) * | 2005-10-14 | 2012-05-03 | Ehrfeld Mikrotechnik Bts Gmbh | Process for the preparation of organic peroxides by microreaction technology |
| CN101298429B (en) * | 2008-05-30 | 2010-10-27 | 浙江时代金科过氧化物有限公司 | Preparation of tert-butyl hydrogen peroxide and di-tert-butyl peroxide |
| CN103627756A (en) * | 2013-11-26 | 2014-03-12 | 江苏科技大学 | Method for enzymatic synthesis of isoquercitrin by using continuous-flow tubular microreactor |
-
2017
- 2017-06-13 CN CN201710442695.2A patent/CN107056670B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN107056670A (en) | 2017-08-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107056670B (en) | A kind of preparation method of two tertiary base peroxide | |
| CN107445808B (en) | Process and system for preparing poly-methoxy-dimethyl ether | |
| CN108863760B (en) | Method for continuously producing glyoxylic acid by using microchannel reactor | |
| CN103755521B (en) | Method for producing KA oil through oxidizing cyclohexane by using air on basis of gas-liquid-solid heterogeneous reaction separation synchronization reactor | |
| CN110496576A (en) | A kind of synthesis of polymethoxy dimethyl ether and separation system | |
| CN102516051B (en) | Method for preparing isophorone by acetone liquid condensation with alkali catalyst | |
| CN103755520A (en) | Method for producing substituted benzyl alcohol, substituted benzaldehyde and substituted benzyl acid through oxidizing substituted methylbenzene with air based on gas-liquid-solid heterogeneous reaction separation synchronization reactor | |
| CN103864587B (en) | A kind of method of synthetic 2-ethyl-2-hexenoic aldehyde | |
| CN106831661B (en) | Method for preparing epoxypropane by using micro-reaction device | |
| CN102260136A (en) | Method for preparing mixture of cyclohexanone and cyclohexanol by oxidazing cyclohexane liquid phase | |
| CN115584284A (en) | Continuous catalytic oxidation-free Fischer-Tropsch wax system and method | |
| CN102050710B (en) | Method for preparing 2-methylacraldehyde and 2-methyl-2-pentenal synchronously | |
| CN108513573A (en) | The manufacturing method and manufacturing device of alkyl nitrite | |
| CN109400480A (en) | A kind of method and apparatus preparing methyl nitrite | |
| CN210646336U (en) | Polyoxymethylene dimethyl ether synthesis and separation system | |
| CN112321530A (en) | Preparation method of continuous synthetic rubber vulcanization accelerator CBS | |
| CN101993374A (en) | Method for preparing C1-C4 alkyl nitrites | |
| CN104709907A (en) | Process and system for selectively removing small amount of H2 from high-concentrations CO gas | |
| CN1693302A (en) | Process for producing methyl carbamate by low pressure solvation homogeneous phase reaction | |
| CN112125774B (en) | Method and device for continuously producing 1, 2-tetrafluoroethane and co-producing glycolic acid | |
| CN109646977A (en) | A kind of reactive distillation coupled and its preparing the application in formic acid | |
| CN103052611B (en) | The preparation method of alpha-methyl styrene | |
| CN217535870U (en) | Device for continuously producing dimethyl sulfoxide | |
| CN115231984B (en) | Process and device for producing alkylbenzene by high-efficiency catalysis and rapid separation of hydrogen fluoride | |
| CN103130653A (en) | Method for continuous production of vinylamine by tubular reactor and device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Preparation method of di-tert-butyl peroxide Effective date of registration: 20200514 Granted publication date: 20190226 Pledgee: Shaanxi Qin Nong rural commercial bank Limited by Share Ltd. hi tech sub branch Pledgor: XI'AN WONDER ENERGY CHEMICAL Co.,Ltd. Registration number: Y2020610000054 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20210618 Granted publication date: 20190226 Pledgee: Shaanxi Qin Nong rural commercial bank Limited by Share Ltd. hi tech sub branch Pledgor: XI'AN WONDER ENERGY CHEMICAL Co.,Ltd. Registration number: Y2020610000054 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: A preparation method of Di tertiary peroxide Effective date of registration: 20210716 Granted publication date: 20190226 Pledgee: Shaanxi Qin Nong rural commercial bank Limited by Share Ltd. hi tech sub branch Pledgor: XI'AN WONDER ENERGY CHEMICAL Co.,Ltd. Registration number: Y2021610000189 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20220726 Granted publication date: 20190226 Pledgee: Shaanxi Qin Nong rural commercial bank Limited by Share Ltd. hi tech sub branch Pledgor: XI'AN WONDER ENERGY CHEMICAL CO.,LTD. Registration number: Y2021610000189 |