CN107459465A - A kind of method for synthesizing diisopropylamine - Google Patents
A kind of method for synthesizing diisopropylamine Download PDFInfo
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- CN107459465A CN107459465A CN201710589199.XA CN201710589199A CN107459465A CN 107459465 A CN107459465 A CN 107459465A CN 201710589199 A CN201710589199 A CN 201710589199A CN 107459465 A CN107459465 A CN 107459465A
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- diisopropylamine
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- UAOMVDZJSHZZME-UHFFFAOYSA-N diisopropylamine Chemical compound CC(C)NC(C)C UAOMVDZJSHZZME-UHFFFAOYSA-N 0.000 title claims abstract description 126
- 229940043279 diisopropylamine Drugs 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 32
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 22
- 239000001257 hydrogen Substances 0.000 claims abstract description 41
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 41
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 41
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000003054 catalyst Substances 0.000 claims abstract description 35
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 20
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 6
- JTPUMZTWMWIVPA-UHFFFAOYSA-O Isopropamide Chemical compound C=1C=CC=CC=1C(C(N)=O)(CC[N+](C)(C(C)C)C(C)C)C1=CC=CC=C1 JTPUMZTWMWIVPA-UHFFFAOYSA-O 0.000 claims abstract description 3
- 229960001737 isopropamide Drugs 0.000 claims abstract description 3
- 239000002808 molecular sieve Substances 0.000 claims description 26
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 26
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 22
- 239000000203 mixture Substances 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000007864 aqueous solution Substances 0.000 claims description 12
- 229910021529 ammonia Inorganic materials 0.000 claims description 11
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 claims description 8
- 239000005049 silicon tetrachloride Substances 0.000 claims description 8
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- 235000019270 ammonium chloride Nutrition 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000005530 etching Methods 0.000 claims description 6
- 238000005342 ion exchange Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000007791 liquid phase Substances 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 claims description 3
- 239000000969 carrier Substances 0.000 claims description 3
- 230000006837 decompression Effects 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 150000002431 hydrogen Chemical class 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 229910001414 potassium ion Inorganic materials 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims description 3
- 239000004408 titanium dioxide Substances 0.000 claims description 3
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 claims description 2
- 229910001863 barium hydroxide Inorganic materials 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 15
- 239000007795 chemical reaction product Substances 0.000 abstract description 8
- 230000015572 biosynthetic process Effects 0.000 abstract description 6
- JJWLVOIRVHMVIS-UHFFFAOYSA-N isopropylamine Chemical compound CC(C)N JJWLVOIRVHMVIS-UHFFFAOYSA-N 0.000 abstract description 5
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 238000009434 installation Methods 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 5
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical compound CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000005576 amination reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 239000002085 irritant Substances 0.000 description 2
- 231100000021 irritant Toxicity 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 206010000087 Abdominal pain upper Diseases 0.000 description 1
- 206010012434 Dermatitis allergic Diseases 0.000 description 1
- 206010012735 Diarrhoea Diseases 0.000 description 1
- 206010028813 Nausea Diseases 0.000 description 1
- 206010037423 Pulmonary oedema Diseases 0.000 description 1
- 229910003978 SiClx Inorganic materials 0.000 description 1
- 206010047700 Vomiting Diseases 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 201000008937 atopic dermatitis Diseases 0.000 description 1
- 208000010668 atopic eczema Diseases 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 231100001231 less toxic Toxicity 0.000 description 1
- 230000008693 nausea Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 208000005333 pulmonary edema Diseases 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000008673 vomiting Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of method for synthesizing diisopropylamine, acetone or isopropanol are used as raw material, are 220~350 DEG C in reaction temperature, pressure is 0.2~1.0MPa of normal pressure, and air speed is 0.5~1.7h with K/ZSM 5 or hydrogen and Ni-based for catalyst‑1Under conditions of react obtained diisopropylamine, carry out aminating reaction synthesizing isopropamide.K/ZSM 5 or hydrogen are used provided by the present invention for the catalyst of synthesis diisopropylamine and Ni-based for catalyst, there is higher diisopropylamine conversion ratio under identical nickel content, the K/ZSM 5 or hydrogen and nickel-base catalyst that the other present invention uses have preferably selectivity, remaining reaction product formation is few, when the K/ZSM 5 of the present invention or hydrogen and nickel-base catalyst are applied into industrial installation, the isopropylamine and isopropanol amount of production system are not further added by, direct circulation by rectification cell without being isolated away, simplify the technological process of production of diisopropylamine, reduce the production cost of diisopropylamine, improve the economic benefit of enterprise.
Description
Technical field
The present invention relates to production low-grade aliphatic amine technical field, specially a kind of method for synthesizing diisopropylamine.
Background technology
Diisopropylamine is colourless transparent liquid, be dissolved in water, ethanol and most of organic solvents, with the smelly volatility liquid of ammonia
Body, the smell for having ammonia, it is volatile, be 84 DEG C in strong basicity, boiling point, freezing point be -96.3 DEG C, it is inflammable, less toxic, be corrosive,
Diisopropylamine is irritant to respiratory tract, suction steam can cause that pulmonary edema, steam be irritant to eye, liquid can cause eye to burn
Wound, skin contact can cause to burn, and can orally cause nausea,vomiting,diarrhea, stomachache, weakness and collapse, and skin contact can draw repeatedly
Rise allergic dermatitis, diisopropylamine is a kind of important organic synthesis intermediate, be widely used in production rubber accelerator, medicine,
Agricultural chemicals, it can also be used to produce surfactant, detergent, defoamer etc., the traditional production method of diisopropylamine has two kinds, and first
Kind it is isopropanol hydrogenation, amination method production diisopropylamine, reaction is divided into two steps, and isopropylamine 27w%, two different is contained in reaction product
Propylamine 33w%, isopropanol 12w%, water 18w%, acetone 7w% etc., reaction product need to can obtain through extraction, rectifying, dehydration rear
Product, second method are acetone hydrogenation, amination diisopropylamine, and reaction is also classified into two steps, contains isopropylamine in reaction product
17w%, diisopropylamine 37w%, isopropanol 20w%, water 10w%, acetone 14w% etc., reaction product are also required to through extraction, essence
Product can just be acquired after step by evaporating, being dehydrated etc., the production method of above two diisopropylamine there is it is identical the shortcomings that：(1)、
Plurality of raw materials participates in reaction, and every kind of raw material is both needed to recycle, complex manufacturing, high energy consumption；(2), reaction product group
Into complicated, separation difficulty, separation process is long, causes unit consumption of product height, product cost high.
The content of the invention
It is an object of the invention to provide a kind of method for synthesizing diisopropylamine, to solve what is proposed in above-mentioned background technology
Problem.
To achieve the above object, the present invention provides following technical scheme：A kind of method for synthesizing diisopropylamine, using acetone
It it is 220~350 DEG C in reaction temperature, pressure is normal with K/ZSM-5 or hydrogen and Ni-based for catalyst or isopropanol is raw material
0.2~1.0MPa is pressed, air speed is 0.5~1.7h-1Under conditions of react obtained diisopropylamine, it is different to carry out aminating reaction synthesis
Propylamine.
Preferably, the K/ZSM-5 catalyst is prepared with the following method：ZSM-5 molecular sieve is taken off first
Aluminium, desiliconization processing, then carry out ion exchange by the ZSM-5 molecular sieve of dealuminzation, desiliconization, are changed into Hydrogen ZSM-5 molecular sieve, most
Generation K/ZSM-5 catalyst is swapped with potassium ion to Hydrogen ZSM-5 molecular sieve afterwards.
Preferably, the K/ZSM-5 catalyst, by weight content meter, containing 40~90% ZSM-5 molecular sieve, 0.5~
3.5% potassium.
Preferably, the dealumination process carries out dealuminzation using vapor or silicon tetrachloride steam.
Preferably, during the use vapor dealuminzation, water vapor pressure is 0.5~10atm, and temperature is 500~650 DEG C,
The dealuminzation time is 3~10h；During using silicon tetrachloride steam dealuminzation, silicon tetrachloride vapor pressure is 0.05~0.3atm, and temperature is
450~630 DEG C, the dealuminzation time is 1.5~4h.
Preferably, the desiliconization uses etching desiliconization, and etching desiliconization uses sodium hydroxide, potassium hydroxide and hydroxide
Any one in the aqueous solution of barium, and 0.05~1.8mol/L of concentration of aqueous solution, temperature are 25~70 DEG C, and desiliconization time is
0.8~2.5h.
Preferably, it is as follows to be changed into Hydrogen ZSM-5 molecular sieve process for the ZSM-5 molecular sieve by dealuminzation, desiliconization：Will be de-
ZSM-5 molecular sieve after aluminium, desiliconization mixes with NH4NO3 or the NH4Cl aqueous solution, and carries out ion exchange, NH4NO3 or
Person NH4Cl concentration of aqueous solution is 0.8~3.5mol/L, 35~70 DEG C, 5~18h of swap time of exchange temperature, exchange times 4
~7 times.
Preferably, the catalyst of the hydrogen and Ni-based composition includes carrier and the active component being supported on carrier, with
The catalyst of the weight and percentage by weight meter of the catalyst of hydrogen and Ni-based composition, hydrogen and Ni-based composition contains 8%~
70% nickel, more than 93% nickel are distributed in carrier surface to the caltalyst of depth 0.7mm hydrogen and Ni-based composition.
Preferably, the preparation method of the hydrogen and Ni-based composition catalyst is：The soluble-salt of active component is dissolved,
Solvent is the mixture of ammoniacal liquor and water, and the weight ratio of ammoniacal liquor and water is 1: 0~0.7, with the spray solution or impregnated carrier of gained,
Then dry, decompose and reduce.
Preferably, the carrier is in aluminum oxide, silica, activated carbon, titanium dioxide or molecular sieve or these carriers
Two or more mixtures.
Preferably, the reacted material is depressurized first, exchange heat cooling, then into the first separator, warp
Hydrogen, ammonia are escaped after decompression from liquid phase, carries out gas-liquid separation herein, liquid phase is stayed in the first separator, and gas is from the
Discharged at the top of one separator, enter the second separator after cooling, be liquefied as liquefied ammonia in this ammonia, stay in the second separator
In, hydrogen is discharged at the top of the second separator.
Compared with prior art, beneficial effects of the present invention are as follows：
K/ZSM-5 or hydrogen are used provided by the present invention for the catalyst of synthesis diisopropylamine and Ni-based for catalyst,
There is higher diisopropylamine conversion ratio under identical nickel content, the K/ZSM-5 that uses of the present invention or hydrogen and Ni-based urge in addition
Agent has preferably selectivity, and remaining reaction product formation is few, by the K/ZSM-5 or hydrogen and nickel-base catalyst of the present invention
During applied to industrial installation, the isopropylamine and isopropanol amount of production system are not further added by, and direct circulation is without passing through
Rectification cell is isolated away, simplifies the technological process of production of diisopropylamine, is reduced the production cost of diisopropylamine, is carried
The economic benefit of Gao Liao enterprises.
Brief description of the drawings
Fig. 1 is each product yield form schematic diagram of the present invention.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained every other under the premise of creative work is not made
Embodiment, belong to the scope of protection of the invention.
Referring to Fig. 1, a kind of method for synthesizing diisopropylamine, uses acetone or isopropanol as raw material, with K/ZSM-5 or hydrogen
Gas and it is Ni-based be catalyst, be 220~350 DEG C in reaction temperature, pressure be 0.2~1.0MPa of normal pressure, air speed for 0.5~
1.7h-1Under conditions of react obtained diisopropylamine, carry out aminating reaction synthesizing isopropamide, K/ZSM-5 catalyst is using such as
It is prepared by lower method：Dealuminzation, desiliconization processing are carried out to ZSM-5 molecular sieve first, then by dealuminzation, the ZSM-5 molecules of desiliconization
Sieve carries out ion exchange, is changed into Hydrogen ZSM-5 molecular sieve, finally swaps life with potassium ion to Hydrogen ZSM-5 molecular sieve
Into K/ZSM-5 catalyst, K/ZSM-5 catalyst, by weight content meter, containing 40~90% ZSM-5 molecular sieve, 0.5~
3.5% potassium, dealumination process carry out dealuminzation using vapor or silicon tetrachloride steam, during using vapor dealuminzation, water vapor pressure
Power is 0.5~10atm, and temperature is 500~650 DEG C, and the dealuminzation time is 3~10h；During using silicon tetrachloride steam dealuminzation, tetrachloro
SiClx steam pressure is 0.05~0.3atm, and temperature is 450~630 DEG C, and the dealuminzation time is 1.5~4h, and desiliconization uses etching
Desiliconization, etching desiliconization is using any one in the aqueous solution of sodium hydroxide, potassium hydroxide and barium hydroxide, and the aqueous solution is dense
0.05~1.8mol/L is spent, temperature is 25~70 DEG C, and desiliconization time is 0.8~2.5h, by dealuminzation, the ZSM-5 molecular sieve of desiliconization
It is as follows to be changed into Hydrogen ZSM-5 molecular sieve process：By the ZSM-5 molecular sieve after dealuminzation, desiliconization with NH4NO3's or NH4Cl
The aqueous solution mixes, and carries out ion exchange, and NH4NO3 or NH4Cl concentration of aqueous solution is 0.8~3.5mol/L, exchange temperature
35~70 DEG C, 5~18h of swap time, exchange times 4~7 times, the catalyst of hydrogen and Ni-based composition includes carrier and is supported on
Active component on carrier, counted with the weight and percentage by weight of hydrogen and the Ni-based catalyst formed, hydrogen and Ni-based composition
Catalyst contain 8%~70% nickel, more than 93% nickel is distributed in carrier surface to depth 0.7mm hydrogen and Ni-based composition
Caltalyst in, hydrogen and it is Ni-based composition catalyst preparation method be：The soluble-salt of active component is dissolved, solvent is
The weight ratio of the mixture of ammoniacal liquor and water, ammoniacal liquor and water is 1: 0~0.7, with the spray solution or impregnated carrier of gained, Ran Hougan
It is dry, decompose and reduce, carrier be in aluminum oxide, silica, activated carbon, titanium dioxide or molecular sieve or these carriers two kinds with
On mixture, reacted material is depressurized first, exchange heat cooling, then into the first separator, after decompression
Hydrogen, ammonia are escaped from liquid phase, carries out gas-liquid separation herein, liquid phase is stayed in the first separator, and gas is from the first separator
Top discharge, enter the second separator after cooling, be liquefied as liquefied ammonia in this ammonia, stay in the second separator, hydrogen from
Discharged at the top of second separator.
In use, K/ZSM-5 or hydrogen are used and Ni-based for catalyst for synthesizing the catalyst of diisopropylamine, identical
There is higher diisopropylamine conversion ratio, the K/ZSM-5 or hydrogen and nickel-base catalyst tool that the present invention uses in addition under nickel content
There is more preferable selectivity, remaining reaction product formation is few, and the K/ZSM-5 of the present invention or hydrogen and nickel-base catalyst are applied to
During industrial installation, the isopropylamine and isopropanol amount of production system are not further added by, and direct circulation is without passing through rectifying list
Member is isolated away, simplifies the technological process of production of diisopropylamine, reduces the production cost of diisopropylamine, improves enterprise
The economic benefit of industry.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of changes, modification can be carried out to these embodiments, replace without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (11)
- A kind of 1. method for synthesizing diisopropylamine, it is characterised in that：Acetone or isopropanol are used as raw material, with K/ZSM-5 or hydrogen Gas and it is Ni-based be catalyst, be 220~350 DEG C in reaction temperature, pressure be 0.2~1.0MPa of normal pressure, air speed for 0.5~ 1.7h-1Under conditions of react obtained diisopropylamine, carry out aminating reaction synthesizing isopropamide.
- A kind of 2. method for synthesizing diisopropylamine according to claim 1, it is characterised in that：The K/ZSM-5 catalyst Prepared with the following method：Dealuminzation, desiliconization processing are carried out to ZSM-5 molecular sieve first, then by dealuminzation, the ZSM- of desiliconization 5 molecular sieves carry out ion exchange, are changed into Hydrogen ZSM-5 molecular sieve, finally Hydrogen ZSM-5 molecular sieve is handed over potassium ion Change generation K/ZSM-5 catalyst.
- A kind of 3. method for synthesizing diisopropylamine according to claim 1, it is characterised in that：The K/ZSM-5 catalyst, Content meter by weight, contain 40~90% ZSM-5 molecular sieve, 0.5~3.5% potassium.
- A kind of 4. method for synthesizing diisopropylamine according to claim 2, it is characterised in that：The dealumination process uses water Steam or silicon tetrachloride steam carry out dealuminzation.
- A kind of 5. method for synthesizing diisopropylamine according to claim 4, it is characterised in that：It is described to use vapor dealuminzation When, water vapor pressure is 0.5~10atm, and temperature is 500~650 DEG C, and the dealuminzation time is 3~10h；Using silicon tetrachloride steam During dealuminzation, silicon tetrachloride vapor pressure is 0.05~0.3atm, and temperature is 450~630 DEG C, and the dealuminzation time is 1.5~4h.
- A kind of 6. method for synthesizing diisopropylamine according to claim 2, it is characterised in that：The desiliconization uses etching Desiliconization, etching desiliconization is using any one in the aqueous solution of sodium hydroxide, potassium hydroxide and barium hydroxide, and the aqueous solution is dense 0.05~1.8mol/L is spent, temperature is 25~70 DEG C, and desiliconization time is 0.8~2.5h.
- A kind of 7. method for synthesizing diisopropylamine according to claim 2, it is characterised in that：It is described by dealuminzation, desiliconization It is as follows that ZSM-5 molecular sieve is changed into Hydrogen ZSM-5 molecular sieve process：By the ZSM-5 molecular sieve and NH4NO3 after dealuminzation, desiliconization Or NH4Cl aqueous solution mixing, and carry out ion exchange, NH4NO3 or NH4Cl concentration of aqueous solution for 0.8~ 3.5mol/L, 35~70 DEG C, 5~18h of swap time of exchange temperature, exchange times 4~7 times.
- A kind of 8. method for synthesizing diisopropylamine according to claim 1, it is characterised in that：The hydrogen and Ni-based composition Catalyst include carrier and the active component that is supported on carrier, with the weight and weight of hydrogen and the Ni-based catalyst formed The catalyst of percentages, hydrogen and Ni-based composition contains 8%~70% nickel, and more than 93% nickel is distributed in carrier surface extremely In the caltalyst of depth 0.7mm hydrogen and Ni-based composition.
- A kind of 9. method for synthesizing diisopropylamine according to claim 1, it is characterised in that：The hydrogen and Ni-based composition The preparation method of catalyst is：The soluble-salt of active component is dissolved, solvent is the mixture of ammoniacal liquor and water, ammoniacal liquor and water Weight ratio is 1: 0~0.7, with the spray solution or impregnated carrier of gained, then dries, decomposes and reduce.
- A kind of 10. method for synthesizing diisopropylamine according to claim 8, it is characterised in that：The carrier be aluminum oxide, Two or more mixture in silica, activated carbon, titanium dioxide or molecular sieve or these carriers.
- A kind of 11. method for synthesizing diisopropylamine according to claim 1, it is characterised in that：The reacted material Depressurized first, exchange heat cooling, then into the first separator, hydrogen, ammonia are escaped from liquid phase after decompression, This carries out gas-liquid separation, and liquid phase is stayed in the first separator, and gas is discharged at the top of the first separator, is entered after cooling Second separator, liquefied ammonia is liquefied as in this ammonia, is stayed in the second separator, hydrogen is discharged at the top of the second separator.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109012741A (en) * | 2018-08-01 | 2018-12-18 | 江苏隆昌化工有限公司 | A kind of method of nano-ZSM-5 molecular sieve catalyst desiliconization |
| CN111056948A (en) * | 2019-12-16 | 2020-04-24 | 中国科学院大连化学物理研究所 | Method for preparing hexamethylenediamine |
| WO2023281081A1 (en) | 2021-07-09 | 2023-01-12 | Spcm Sa | Method for obtaining bio-sourced substituted alkyl(meth)acrylamide |
| CN115819246A (en) * | 2022-11-30 | 2023-03-21 | 中国科学院大连化学物理研究所 | A kind of preparation method of diisopropylamine |
| CN116173995A (en) * | 2021-11-29 | 2023-05-30 | 安徽昊源化工集团有限公司 | Catalyst for preparing morpholine by diethylene glycol method and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109012741A (en) * | 2018-08-01 | 2018-12-18 | 江苏隆昌化工有限公司 | A kind of method of nano-ZSM-5 molecular sieve catalyst desiliconization |
| CN109012741B (en) * | 2018-08-01 | 2021-09-03 | 江苏隆昌化工有限公司 | Method for desiliconizing nano ZSM-5 molecular sieve catalyst |
| CN111056948A (en) * | 2019-12-16 | 2020-04-24 | 中国科学院大连化学物理研究所 | Method for preparing hexamethylenediamine |
| WO2023281081A1 (en) | 2021-07-09 | 2023-01-12 | Spcm Sa | Method for obtaining bio-sourced substituted alkyl(meth)acrylamide |
| FR3125042A1 (en) | 2021-07-09 | 2023-01-13 | Snf Sa | Process for obtaining biosourced substituted alkyl(meth)acrylamide |
| CN116173995A (en) * | 2021-11-29 | 2023-05-30 | 安徽昊源化工集团有限公司 | Catalyst for preparing morpholine by diethylene glycol method and preparation method thereof |
| CN115819246A (en) * | 2022-11-30 | 2023-03-21 | 中国科学院大连化学物理研究所 | A kind of preparation method of diisopropylamine |
| CN115819246B (en) * | 2022-11-30 | 2024-03-19 | 中国科学院大连化学物理研究所 | A kind of preparation method of diisopropylamine |
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Application publication date: 20171212 |