CN207929218U

CN207929218U - CH based on minute bubbles reaction kettle3Cl synthesizers

Info

Publication number: CN207929218U
Application number: CN201820146142.2U
Authority: CN
Inventors: 余家骧
Original assignee: Individual
Current assignee: Individual
Priority date: 2018-01-29
Filing date: 2018-01-29
Publication date: 2018-10-02
Anticipated expiration: 2028-01-29

Abstract

The utility model is a kind of CH based on minute bubbles reaction kettle₃Cl synthesizers, it includes graphite cooler, diluted acid water pump, aerosol feeding equipment and static mixer, its main feature is that：Further include minute bubbles reaction kettle, the gas vent on minute bubbles reaction kettle top and the thick CH of graphite cooler₃The connection of Cl entrances, side liquid inlet connected by the outlet of diluted acid water pump and graphite cooler, first L-type sealed end of minute bubbles reaction kettle is connect with aerosol feeding equipment, second L-type sealed end of minute bubbles reaction kettle is connect with static mixer, first outlet is set between diluted acid water pump and the liquid inlet of minute bubbles reaction kettle side, second outlet, the thick CH of graphite cooler are being set at diluted acid water pump₃Cl is exported and CH₃The refined unit of Cl connects, and the water inlet of graphite cooler is connect with cooling upper water, water outlet is connect with cooling lower water.

Description

CH based on minute bubbles reaction kettle3Cl synthesizers

Technical field

The utility model is related to chemical industry equipments, and in particular to CH₃Cl is synthesized, and is a kind of CH based on minute bubbles reaction kettle₃Cl Synthesizer.

Background technology

The CH of the prior art₃Cl synthesizers, reaction kettle shell are steel lining polytetrafluoroethylene (PTFE), and upper layer bubbling pipe passes through the One L-type sealed end and CH₃OH steam pipe lines connect, and lower layer's bubbling pipe is connect by the second L-type sealed end with HCl gas lines. Due to CH₃Dimethyldichlorosilane containing 26~14mmHg partial pressures in Cl (is commonly called as M₂), rapid hydrolysis at high temperature generates poly- silicon Oxygen alkane can block the aperture on bubbling pipe, therefore, be bubbled the hole that can only bore φ 10mm on tube wall, lead to the thick of reactor product CH₃Contain 3~5% dimethyl ether CH in Cl gases₃OCH₃, see Fig. 1.

Invention content

Technical problem to be solved in the utility model is：The shortcomings that overcoming the prior art provides a kind of minute bubbles CH₃Cl Synthesis reaction vessel, with the method for the patent of invention ZL201410012358.8 of Granted publication on January 27th, 2016, by raw material HCl By freezing+absorption by M₂Recycling is purified, and P M are reached₂＜ 0.2mmHg can prevent from being bubbled blockage, to reduce drum The aperture of pipe is steeped, increases gas liquid interfacial area, reduces the thick CH of reactor product₃CH in Cl gases₃OCH₃Content.

The utility model solve technical problem scheme be：A kind of CH based on minute bubbles reaction kettle₃Cl synthesizers, it Including graphite cooler, diluted acid water pump, aerosol feeding equipment and static mixer, it is characterized in that：It further include minute bubbles reaction Kettle, the gas vent on minute bubbles reaction kettle top and the thick CH of graphite cooler₃Cl entrances connection, side liquid inlet It is connected by the outlet of diluted acid water pump and graphite cooler, the first L-type sealed end of minute bubbles reaction kettle passes through PVC threeways and gas Colloidal sol feeding equipment connect and by aerosol feeding equipment respectively with HCl gas lines and liquid CH₃OH pipelines connect, small Second L-type sealed end of bubble reaction kettle connect with static mixer and by static mixer respectively with CH₃OH steam pipe lines Connected with HCl gas lines, between diluted acid water pump and the liquid inlet of minute bubbles reaction kettle side setting for diluted acid water with M₂The second outlet for extra diluted acid water to be discharged, stone is being arranged in the first outlet of hydrolysis unit connection at diluted acid water pump The thick CH of black cooler₃Cl is exported and CH₃The refined unit of Cl connects, and the water inlet of graphite cooler connect with cooling upper water, goes out The mouth of a river is connect with cooling lower water.

The CH based on minute bubbles reaction kettle₃Two diluted acid water injection pipes, one diluted acid is arranged in Cl synthesizers Water injection pipe one end is connect by PVC threeways with the vertical tube of the first L-type sealed end of minute bubbles reaction kettle simultaneously, another diluted acid Water injection pipe is connect with the vertical tube of the second L-type sealed end, and the other end of two diluted acid water injection pipes connects with diluted acid water pipeline simultaneously It connects.

The minute bubbles reaction kettle includes shell, upper layer bubbling pipe, lower layer's bubbling pipe, the first L-type sealed end and the second L-type Sealed end, the top setting gas vent of the shell, side are arranged liquid inlet, the upper layer bubbling pipe is placed in shell, Below liquid inlet, lower layer's bubbling pipe is placed in shell, below the bubbling pipe of upper layer, and the first L-type sealed end is placed in shell External side, transverse tube are connect outside shell with upper layer bubbling pipe, and the second L-type sealed end is placed in hull outside, transverse tube in shell It is connect outside with lower layer bubbling pipe.

The upper layer bubbling pipe is identical as lower layer's bubbling pipe structure and connection relation, and structure is：It includes header, envelope Plug, bubbling pipe, the header are arranged one as the transverse tube of the first L-type sealed end or the transverse tube of the second L-type sealed end Import and several outlets, the vertical tube of the import of header and the first L-type sealed end or the vertical tube of the second L-type sealed end be connected, Several outlets are respectively connected with the bubbling pipe, and the other end of bubbling pipe blocks, and on upper layer, bubbling pipe sets along Zhou Guanbi Set several a diameter of d₁Aperture, several a diameter of d are set along Zhou Guanbi in lower layer's bubbling pipe₂Aperture.

The aperture d of the upper layer bubbling pipe₁With the aperture d of lower layer bubbling pipe₂Relationship be：

The aerosol feeding equipment includes three runner atomizers and double taper pipe, structure are：Three runner atomizers include Steel threeway, polytetrafluoroethylene (PTFE) double taper pipe, liquid CH₃OH pipes, HCl central tubes, steel threeway one end passes through PVC threeways and first Vertical tube connection, the other end and the metal blind plate of L-type sealed end are connected, medial inlet and HCl gas lines are tightly connected, described poly- Tetrafluoroethene double taper pipe is placed in PVC threeways, the liquid CH₃It is stretched into after the front end necking down of OH pipes in steel threeway and polytetrafluoroethylene (PTFE) Double taper pipe with one heart, rear end and liquid CH₃OH pipelines are tightly connected, and one of steel flange is connected with metal blind plate, liquid CH₃OH Pipe welds after being adjusted to correct position；Before this, its end of HCl central tubes flashed liquid CH₃OH pipes are outer, after welding again Package liquid CH₃The necking down pipe of OH pipes front end, the HCl central tubes of necking down, the liquid CH of necking down₃OH pipe spout turning is evened up, so Afterwards and polytetrafluoroethylene (PTFE) double taper pipe with one heart, between form concentric center flowing hole, interior overcurrent annulus and outer overcurrent annulus, jointly Constitute aerosol feeding equipment.

The technical process of the utility model is：

1 purified feed stock HCl, by the raw material HCl patents of invention of the January in 2016 of Granted publication on the 27th The method of ZL201410012358.8, by freezing+absorption by M therein₂Recovery purifying reaches P M₂＜ 0.2mmHg；

2 first open lower layer's bubbling pipe, are passed through the gas phase HCl being uniformly mixed through static mixer and gas phase CH₃The mixing of OH Gas begins to warm to 140 DEG C with 50% load, then opens upper layer bubbling pipe, increases liquid CH₃The amount of OH keeps HCl： CH₃OH=1.1~1.15, when upper layer load ＞ 70%, system stablize when between 130 DEG C~140 DEG C, if larger fluid CH₃OH Inlet amount, so that temperature is declined, vice versa；

3 generations contain CH₃OCH₃The thick CH of ＜ 0.3%₃Cl is passed through thick by the gas vent on minute bubbles reaction kettle top CH₃Cl entrances enter graphite cooler, are exchanged with the cooling water heat of graphite cooler, after reducing temperature, by thick CH₃Cl outlet streams Go out graphite cooler, into CH₃The refined unit of Cl；

When 4 shutdown of short term, diluted acid is injected into the vertical tube of the vertical tube of the first L-type sealed end and the second L-type sealed end immediately Water so that when the temperature drops, without ZnCl₂Crystallization be precipitated, prevent ZnCl₂Crystallization precipitation cause be bubbled hole plug.

The utility model has the beneficial effects that：

1 the utility model uses aerosol feeding equipment, using gas phase CH₃OH and liquid phase CH₃OH is fed respectively, liquid phase CH₃OH is atomized by three runner atomizers, makes liquid CH₃OH droplets suspend in the gas phase, and droplet can when suspending in " aerosol " Pass through liquid CH₃Reaction heat is taken out in the evaporation of OH, makes catalyst Z nCl₂Solution temperature is stablized, and can save most of liquid phase CH₃OH vaporizes required steam, energy saving；Gas phase CH₃OH can utilize CH₃Cl synthesising reacting heats make system gradually heat up； And gas phase CH can be passed through₃OH, liquid phase CH₃OH feeds to control charging CH respectively₃The liquid of OH, gas ratio, and then control this reality With the thermal balance of novel reaction kettle；

The upper layer bubbling pipe of 2 the utility model is passed through gas phase HCl and liquid CH₃The aerosol of OH, lower layer's bubbling pipe are passed through The gas phase HCl and gas phase CH being uniformly mixed through static mixer₃The gaseous mixture of OH, it can be ensured that containing enough in each minute bubbles HCl and CH₃OH is reacted, it is ensured that after stingy follicular rupture, CH₃OCH₃＜ 0.3%；

The aperture d of the upper layer bubbling pipe of 3 the utility model₁With the aperture d of lower layer bubbling pipe₂ Item Under part, the CH in the aerosol bubble of upper layer bubbling pipe₃After OH evaporations, volume increases nearly 1 times so that the bubble of two rows is straight Diameter is identical；

According to An Tuo Britain side journey,Calculate P M when different temperatures₂For

Temperature DEG C	-10℃	-15℃	-20℃	-60℃
					PM₂㎜Hg	26.46	20.01	14.98	0.902

T=273.3-t

And d₁Or d₂The aperture of=2~3 ㎜ makes gas liquid interfacial area increase 3~5 times, single isolated bubbles center to bubble interface Concentration gradient also increase 3~5 times, therefore in HCl ＞ CH₃When the bubbles burst of OH, CH₃OCH₃＜ 0.3%；

Raw material HCl used in 4 the utility model passes through the patent of invention with the January in 2016 of Granted publication on the 27th The method of ZL201410012358.8 is purified, by raw material HCl by freezing+absorption by M₂Recycling, reaches P M₂＜ 0.2mmHg had both recycled valuable M₂, also ensure that being bubbled bore dia will not block small 2 ㎜ to φ；

Diluted acid is respectively arranged on the vertical tube of the first L-type sealed end and the vertical tube of the second L-type sealed end in 5 the utility model The structure of water injection pipe, can in temporary parking, when the temperature drops, preventing ZnCl₂Crystallization precipitation cause be bubbled hole plug.

Description of the drawings

Fig. 1 is the CH of the prior art₃The structural schematic diagram of Cl synthesizers；

Fig. 2 is CH of the utility model based on minute bubbles reaction kettle₃The structural schematic diagram of Cl synthesizers；

Fig. 3 is CH of the utility model based on minute bubbles reaction kettle₃The structure of three runner atomizers of Cl synthesizers is shown It is intended to；

Fig. 4 is the K close-up schematic views of Fig. 3.

In figure：1CH₃OH steam pipe lines, 2HCl gas lines, 3 thick CH₃Cl is exported, 4 temperature adjustments diluted acid water, 5 diluted acid water, and 6 Extra diluted acid water, 7 thick CH₃Cl synthesis gas, the upper water of 8 coolings, the lower water of 9 coolings, 10 liquid CH₃OH pipelines, 11 first L-type sealed ends, 12 second L-type sealed ends, 13 diluted acid water injection pipes, 14 upper layer bubbling pipes, 15 lower layer's bubbling pipes, 16 metal blind plates, 17 steel flanges, 18PVC threeways, 19 polytetrafluoroethylene (PTFE) double taper pipes, 20 steel threeways, 21HCl central tubes, 22 liquid CH₃OH is managed, 23 outer overcurrent annulus, Overcurrent annulus in 24,25 center flowing holes, 101 minute bubbles reaction kettles, 102 graphite coolers, 103 diluted acid water pumps, 104 is static mixed Clutch, 105 aerosol feeding equipments.

Specific implementation mode

The utility model is further illustrated with reference to the accompanying drawings and examples.

With reference to Fig. 2~Fig. 4, embodiment 1, a kind of CH based on minute bubbles reaction kettle of the present embodiment₃Cl synthesizers, it is wrapped Graphite cooler 102, diluted acid water pump 103, aerosol feeding equipment 105 and static mixer 104 are included, further includes minute bubbles reaction Kettle 101, the thick CH of the gas vent and graphite cooler 102 on 101 top of minute bubbles reaction kettle₃The connection of Cl entrances, side Liquid inlet connect with the outlet of graphite cooler 102 by diluted acid water pump 103, it is stingy for injecting temperature adjustment diluted acid water 4 First L-type sealed end 11 of bubble reaction kettle 101 is connect with aerosol feeding equipment 105 by PVC threeways 18 and passes through aerosol Feeding equipment 105 respectively with HCl gas lines 2 and liquid CH₃OH pipelines 10 connect, and the second L-type of minute bubbles reaction kettle 101 is close Sealing end 12 connect with static mixer 104 and by static mixer 104 respectively with CH₃OH steam pipe lines 1 and HCl flues Line 2 connects, and setting is for diluted acid water 5 and M between the liquid inlet of 101 side of diluted acid water pump 103 and minute bubbles reaction kettle₂Water The second outlet for extra diluted acid water 6 to be discharged, stone is being arranged in the first outlet for solving unit connection at diluted acid water pump 103 The thick CH of black cooler 102₃Cl exports 3 and CH₃The refined unit of Cl connects, the water inlet of graphite cooler 102 and cooling upper water 8 connections, water outlet are connect with cooling lower water 9.

The CH based on minute bubbles reaction kettle₃Two diluted acid water injection pipes 13 are arranged in Cl synthesizers, one dilute 13 one end of sour water injection pipe passes through the vertical tube of PVC threeways 18 and the first L-type sealed end 11 of the minute bubbles reaction kettle 101 simultaneously Connection, another diluted acid water injection pipe 13 connect with the vertical tube of the second L-type sealed end 12, two diluted acid water injection pipes 13 it is another End is connect with diluted acid water pipeline.

The minute bubbles reaction kettle 101 includes shell, upper layer bubbling pipe 14, lower layer's bubbling pipe 15, the first L-type sealed end 11 With the second L-type sealed end 12, liquid inlet, the upper layer bubbling pipe is arranged in the top setting gas vent of the shell, side 14 are placed in shell, below liquid inlet, and lower layer's bubbling pipe 15 is placed in shell, 14 lower section of upper layer bubbling pipe, and described the One L-type sealed end 11 is placed in hull outside, transverse tube and is connect with upper layer bubbling pipe 14 outside shell, the second L-type sealed end 12 Hull outside, transverse tube is placed in connect with lower layer bubbling pipe 15 outside shell.

The upper layer bubbling pipe 14 is identical as 15 structure of lower layer bubbling pipe and connection relation, and structure is：It includes afflux Pipe, block head, bubbling pipe, the header as the transverse tube of the first L-type sealed end 11 or the transverse tube of the second L-type sealed end 12, An import and several outlets, the vertical tube or the second L-type sealed end of the import of header and the first L-type sealed end 11 is arranged in it 12 vertical tube is connected, several outlets are respectively connected with the bubbling pipe, and the other end of bubbling pipe blocks, in upper layer bubbling pipe 14 along Zhou Guanbi are arranged several a diameter of d₁Aperture, it is a diameter of that along Zhou Guanbi several are set in lower layer's bubbling pipe 15Aperture.

The aerosol feeding equipment 105 includes three runner atomizers and double taper pipe, structure are：Three runner atomizer packets Include steel threeway 20, polytetrafluoroethylene (PTFE) double taper pipe 19, liquid CH₃OH pipes 22, HCl central tubes 21, described 20 one end of steel threeway pass through PVC threeways 18 connect with the vertical tube of the first L-type sealed end 11, the other end and metal blind plate 16 are connected, medial inlet and HCl gases Pipeline 2 is tightly connected, and the polytetrafluoroethylene (PTFE) double taper pipe 19 is placed in PVC threeways 18, the liquid CH₃The 22 front end necking down of OH pipes After stretch into steel threeway 20 with polytetrafluoroethylene (PTFE) double taper pipe 19 is concentric, rear end and liquid CH₃22 line 10 of OH pipes is tightly connected, wherein One steel flange 17 is connected with metal blind plate 16, liquid CH₃OH pipes 22 weld after being adjusted to correct position；Before this, described Its end of HCl central tubes 21 flashed liquid CH₃Outside OH pipes 22, liquid CH is packaged after welding again₃The necking down pipe of 22 front end of OH pipes, The HCl central tubes 21 of necking down, the liquid CH of necking down₃The 22 spout turning of OH pipes is evened up, then same with polytetrafluoroethylene (PTFE) double taper pipe 19 The heart, between form concentric center flowing hole 25, interior overcurrent annulus 24 and outer overcurrent annulus 23, collectively form aerosol charging dress Set 105.

The present embodiment is manufactured using the prior art.

The technical process of the present embodiment is：

1 purified feed stock HCl, by the raw material HCl patents of invention of the January in 2016 of Granted publication on the 27th The method of ZL201410012358.8 is purified, by freezing+absorption by M therein₂Recycling, reaches P M₂＜ 0.2mmHg；

2 first open lower layer's bubbling pipe 15, are passed through the gas phase HCl being uniformly mixed through static mixer 104 and gas phase CH₃OH's Gaseous mixture begins to warm to 140 DEG C with 50% load, then opens upper layer bubbling pipe 14, increases liquid CH₃The amount of OH is protected Hold HCl：CH₃OH=1.1~1.15, when upper layer load ＞ 70%, system stablize when between 130 DEG C~140 DEG C, larger fluid CH₃The inlet amount of OH makes temperature in bed decline, and vice versa；

3 generations contain CH₃OCH₃The thick CH of ＜ 0.3%₃Cl synthesis gas 7 by 101 top of minute bubbles reaction kettle gas vent Pass through thick CH₃Cl entrances enter graphite cooler 102, are exchanged with the cooling water heat of graphite cooler 102, after reducing temperature, by Thick CH₃3 outflow graphite coolers 102 of the outlets Cl, into CH₃The refined unit of Cl；

It is close to the vertical tube of the first L-type sealed end 11 and the second L-type by diluted acid water injection pipe 13 immediately when 4 shutdown of short term The vertical tube of sealing end 12 injects diluted acid water so that when the temperature drops, without ZnCl₂Crystallization be precipitated, prevent ZnCl₂Crystallization be precipitated Cause to be bubbled hole plug.

The present embodiment directly achieves recycling M₂89.5-127kg/h, CH3Cl4800-8000 tons are produced every year and per small more When save steam 11.1-1.36 ton hours economic benefit.

The utility model is not limited to present embodiment, to those skilled in the art, without creativeness The simple copy and improvement of labour belong to the range that the utility model claims are protected.

Claims

1. a kind of CH based on minute bubbles reaction kettle₃Cl synthesizers, it includes graphite cooler, diluted acid water pump, aerosol charging Device and static mixer, it is characterized in that：Further include minute bubbles reaction kettle, the gas vent on minute bubbles reaction kettle top with The thick CH of graphite cooler₃Cl entrances connect, the liquid inlet of side is connected by the outlet of diluted acid water pump and graphite cooler, First L-type sealed end of minute bubbles reaction kettle is connect with aerosol feeding equipment by PVC threeways and is fed by aerosol and filled Set respectively with HCl gas lines and liquid CH₃OH pipelines connect, the second L-type sealed end and static mixing of minute bubbles reaction kettle Device connect and by static mixer respectively with CH₃OH steam pipe lines are connected with HCl gas lines, diluted acid water pump with it is stingy Setting is used for diluted acid water and M between steeping the liquid inlet of reaction kettle side₂The first outlet of hydrolysis unit connection, close to diluted acid Second outlet for extra diluted acid water to be discharged, the thick CH of graphite cooler are set at water pump₃Cl is exported and CH₃The refined list of Cl Member connection, the water inlet of graphite cooler is connect with cooling upper water, water outlet is connect with cooling lower water.

2. the CH as described in claim 1 based on minute bubbles reaction kettle₃Cl synthesizers, it is characterized in that：It is described to be based on minute bubbles The CH of reaction kettle₃Two diluted acid water injection pipes are arranged in Cl synthesizers, and one diluted acid water injection pipe one end passes through PVC simultaneously Threeway is connect with the vertical tube of the first L-type sealed end of minute bubbles reaction kettle, another diluted acid water injection pipe and the second L-type sealed end Vertical tube connection, the other ends of two diluted acid water injection pipes connect with diluted acid water pipeline simultaneously.

3. the CH as described in claim 1 based on minute bubbles reaction kettle₃Cl synthesizers, it is characterized in that：The minute bubbles reaction Kettle includes shell, upper layer bubbling pipe, lower layer's bubbling pipe, the first L-type sealed end and the second L-type sealed end, the top of the shell Gas vent, side setting liquid inlet are set, and the upper layer bubbling pipe is placed in shell, below liquid inlet, the lower layer Bubbling pipe is placed in shell, below the bubbling pipe of upper layer, the first L-type sealed end be placed in hull outside, transverse tube outside shell with The connection of upper layer bubbling pipe, the second L-type sealed end are placed in hull outside, transverse tube and are connect with lower layer bubbling pipe outside shell.

4. the CH as claimed in claim 3 based on minute bubbles reaction kettle₃Cl synthesizers, it is characterized in that：The upper layer bubbling pipe Identical as lower layer's bubbling pipe structure and connection relation, structure is：It includes header, block head, bubbling pipe, the header As the transverse tube of the first L-type sealed end or the transverse tube of the second L-type sealed end, an import and several outlets, afflux are set The vertical tube of the import of pipe and the first L-type sealed end or the vertical tube of the second L-type sealed end be connected, several outlets respectively with it is described Bubbling pipe is connected, and the other end of bubbling pipe blocks, and on upper layer, bubbling pipe is arranged several a diameter of d along Zhou Guanbi₁Aperture, Several a diameter of d are set along Zhou Guanbi in lower layer's bubbling pipe₂Aperture.

5. the CH as claimed in claim 4 based on minute bubbles reaction kettle₃Cl synthesizers, it is characterized in that：The upper layer bubbling pipe Aperture d₁With the aperture d of lower layer bubbling pipe₂Relationship be：

6. the CH as described in claim 1 based on minute bubbles reaction kettle₃Cl synthesizers, it is characterized in that：The aerosol charging Device includes three runner atomizers and double taper pipe, structure are：Three runner atomizers include steel threeway, polytetrafluoroethylene (PTFE) bipyramid Pipe, liquid CH₃OH pipes, HCl central tubes, steel threeway one end connect by PVC threeways with the vertical tube of the first L-type sealed end, The other end is connected with metal blind plate, medial inlet and HCl gas lines are tightly connected, and the polytetrafluoroethylene (PTFE) double taper pipe is placed in In PVC threeways, the liquid CH₃Stretched into after the front end necking down of OH pipes in steel threeway with polytetrafluoroethylene (PTFE) double taper pipe is concentric, rear end and Liquid CH₃OH pipelines are tightly connected, and one of steel flange is connected with metal blind plate, liquid CH₃After OH pipes are adjusted to correct position It welds；Before this, its end of HCl central tubes flashed liquid CH₃OH pipes are outer, package liquid CH after welding again₃OH pipes front end Necking down pipe, the HCl central tubes of necking down, the liquid CH of necking down₃OH pipe spouts are evened up, then same with polytetrafluoroethylene (PTFE) double taper pipe The heart, between form concentric center flowing hole, interior overcurrent annulus and outer overcurrent annulus, collectively form aerosol feeding equipment.