CN202122957U - Multistage acidification reactor for continuous production of formic acid - Google Patents
Multistage acidification reactor for continuous production of formic acid Download PDFInfo
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- CN202122957U CN202122957U CN2011202010866U CN201120201086U CN202122957U CN 202122957 U CN202122957 U CN 202122957U CN 2011202010866 U CN2011202010866 U CN 2011202010866U CN 201120201086 U CN201120201086 U CN 201120201086U CN 202122957 U CN202122957 U CN 202122957U
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- kettle
- formic acid
- end plate
- collection case
- multistage
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Abstract
The utility model discloses a multistage acidification reactor for continuous production of formic acid, which comprises a closed kettle enclosed by a left end plate, a right end plate, an upper barrel and a lower barrel. Heating jackets are disposed in fore-aft symmetry on the outer lower portion and in the outer middle of the kettle, an internal condenser is axially hung on the upper portion of the interior of the kettle through a holder, a coolant inlet pipe and a coolant outlet pipe of the internal condenser are led out of the upper portion of the left end plate and the upper portion of the right end plate respectively, a premixing material inlet pipe is disposed on the lower portion of the left end plate, and a reaction liquid outlet pipe on the lower portion of the right end of the kettle penetrates through the kettle to be led out of the heating jackets. The multistage acidification reactor with the integrated structure is low in equipment investment. The multistage acidification reactor with a membrane type wall heating structure is higher in heat transferring efficiency and better in structural strength. Energy is more reasonably utilized, operation varies in chambers according to change of systematic viscidity, reaction of materials can be exactly completed from an inlet to an outlet, intermediate links are reduced by means of continuous operation, operation is simplified, efficiency is higher, and the multistage acidification reactor is applicable to mass production.
Description
Technical field
The utility model relates to a kind of stage acidizing reaction unit, particularly relates to a kind of formic acid quantity-produced stage acidizing reaction unit that is used for.
Background technology
Formic acid belongs to basic Organic Chemicals, be acid stronger a kind of in the aliphatic carboxylic acid, and have some chemical property of aldehyde, so purposes is more, is widely used in industries such as medicine, agricultural chemicals, leather, dyestuff, rubber, metallurgy and food.Formic acid production mainly contains butane (or light oil) liquid phase oxidation, formamide method, methyl formate hydrolysis method and four kinds of process routes of sodium formate acidization in the industry.Wherein butane (or light oil) liquid phase oxidation technique is a kind of production method of producing acetic acid coproduction simultaneously formic acid; 1 ton of acetate of every production; 0.05～0.25 ton of formic acid of by-product; Once be the main method of producing formic acid abroad the seventies in last century, afterwards along with the industrialization of synthesizing acetic acid by methanol low-pressure carbonylation technology, makes this method lose development prospect; The formamide method is because of long flow path, raw material are complicated, production cost is high, and also be eliminated the eighties in last century; The methyl formate hydrolysis method is the main method that external formic acid is produced; Be characterized in only consuming carbon monoxide and water, produce single formic acid, no coupling product; But this method relates to complicated petrochemical process and separation process; And receive the violent influence that goes up of petrochemical materials price, more important is that one-time investment is higher, is not suitable for domestic formic acid manufacturing enterprise.The sodium formate acidization is adopted in present domestic formic acid production mostly, and this method is acidulant with sulfuric acid traditionally, and production process will consume a large amount of sulfuric acid, and the sodium sulphate product price of by-product is cheap in addition, and therefore comparing the methyl formate hydrolysis method lacks competitiveness.But because sodium formate can be produced by carbon monoxide and caustic soda reaction; And carbon monoxide is rich in a large amount of tail gas of chemical industry, metallurgical industry; Therefore the technology that the carbon monoxide tail gas recycle is combined with formic acid production just should need and give birth to; Particularly after " yellow phosphorus industry access condition " released, just shone vitality based on the sodium formate acidifying system formic acid method that the yellow phosphoric tail gas resource is recycled.
Yellow phosphoric tail gas is the gaseous products that the rock phosphate in powder electric furnace smelting produces, and wherein the mass fraction of carbon monoxide is about 90%, and all the other mainly are that sulfide, phosphide and ash grade.Because purifying exhausting gas of yellow phosphorus is difficult, mostly directly burning and exhausting caused a large amount of energy wastes in the past.Generally, 1 ton of yellow phosphorus of every production produces 2800m approximately
3Tail gas.With 2008 be example, the actual production capacity 8.24x10 of national yellow phosphorus
5Ton, about 22.3 billion cubic meters of discharging tail gas, directly combustion row just means has wasted 23.5x10
16The heat energy of J, the objective requirement of do not meet energy-conserving and environment-protective, developing a circular economy.So the resource recovery and utilization technology to yellow phosphoric tail gas is just brought into schedule; Except that utilizing the tail gas heat quantity dried material, firing hot water or the byproduct steam generating; Sodium formate is produced in tail gas and caustic soda reaction through deep purifying; Formic acid is produced in acidifying to sodium formate again, has become the mainstream technology that current yellow phosphoric tail gas resource reclaims.According to the difference of acidulant, the distinct methods with phosphoric acid,diluted, peroxophosphoric acid, polyphosphoric acid acidifying sodium formate has appearred at present.But in comparison, because of concentration, the purity of polyphosphoric acid acidifying formic acid that sodium formate is produced are higher, added value of product is bigger, and is therefore more competitive.
Utilizing the polyphosphoric acids acidifying sodium formate to produce high-quality formic acid, is under uniform temperature condition and acidification adjuvant condition, utilizes first hydrionic chemical energy double decomposition sodium formate in the acid, makes it to be converted into formic acid and mainly contains NaH
2PO
4The compound phosphoric acid sodium salt.Carry out the separation of formic acid after reaction is accomplished again with the distillation mode, promptly obtain concentration formic acid and high after the condensation, and solid product compound phosphoric acid sodium salt can be regulated its pH value through adding aqueous slkali, carry out polymerisation afterwards again and generate sodium phosphate trimer.In the implementation procedure of a whole set of technology, acidification reaction is the most key, and reaction temperature, reaction pressure, reaction time and proportioning raw materials etc. all can influence the quality and the yield of formic acid, and then the device of accomplishing acidification reaction has been proposed requirements at the higher level.
In sodium formate and the polyphosphoric acid course of reaction, system viscosity changes, unusual thickness during beginning, and along with the carrying out of reaction, viscosity diminishes, and this mainly is because the formic acid of producing is better mobile.But formic acid has volatility, and because reaction temperature and its boiling point are approaching, is attended by the formic acid vaporization, and this just means that course of reaction must control the content of formic acid in the system, keeps certain fluidity, fully carries out otherwise reaction is very difficult.Therefore, the polyphosphoric acid acidifying sodium formate serialization device of producing formic acid must meet the following conditions simultaneously: want (1) can adaptive response process system viscosity change and provide rational and effective to stir; (2) want can the hierarchy of control in the content of formic acid, promptly the formic acid to volatilization or vaporization can carry out in time replenishing; (3) want effective heating mode can be provided, create stable reaction temperature environment; (4) to have the function of continued operation, just react completely from being fed to discharging.But existing mostly intermittently operated of various consersion units through reinforced again after the reaction time, reaction again, so back and forth, is not suitable for large-scale production.In existing each patent about sodium formate acidifying system formic acid; Mostly used acidizing device is not introduced; Only patent 200710078073.2 is mentioned and is adopted commercially available RDS-0.05 type cone-shaped reactor moment to carry out the acidification reaction of sodium formate; But do not introduce apparatus structure, also undeclared is how to satisfy aspects such as system viscosity, temperature and successive reaction to require.
Summary of the invention
The purpose of the utility model is to provide a kind of formic acid quantity-produced stage acidizing reaction unit that is used for; Be formic acid production to be reclaimed with the yellow phosphoric tail gas resource combine; On suitable temperature environment and the basis that efficiently mixes, the serialization production of the completion formic acid of ability low-consumption high-efficiency.
The utility model solves the technical scheme that its technical problem adopted:
The utility model comprises the sealing kettle that is surrounded jointly by first member plate, right end plate, upper shell, middle cylinder body, lower shell; Symmetric arrangement has heating jacket before and after kettle outer lower portion and the outside central region; The kettle inside upper part has hung built-in condenser through fixed mount along axis; The refrigerant inlet tube and the refrigerant exit pipe of built-in condenser are drawn through the top of first member plate and right end plate respectively; Premix feed(raw material)inlet pipe is arranged in the first member plate bottom, and the reactant liquor outlet of kettle right-hand member bottom passes heating jacket from kettle and draws.
Described kettle is divided into a plurality of reative cells by dividing plate, dividing plate quantity, spacing, adjustable height, and each reative cell all disposes different agitators according to the regional viscosity difference of the system that becomes sticky.
Described built-in condenser is one another in series by refrigerant inlet tube, refrigerant inlet collection case, condensation tube bank, refrigerant exit collection case and refrigerant exit pipe and is welded, and wherein refrigerant inlet collection case and refrigerant exit collection case have the anti-corrosion steel pipe formation in the hole that is used for inserting the condensation tube bank by closed at both ends and side.
Described heating jacket adopts membrane wall structure; Be welded jointly by two the heating agent inlet tubes in top, two heating agent inlet collection casees, a plurality of false add heat pipe, bottom heating agent outlet collection case and heating agent outlets, wherein the false add heat pipe bends according to the external diameter of lower shell.
Compared to all types of stirring reaction devices of routine, the completion polyphosphoric acid that the utility model can be flexible and efficient creates conditions for producing high-quality formic acid to the acidification reaction of sodium formate, and it has effect and is embodied in:
(1) adopts systematization, integrated structural design pattern.This acidification reaction device is integrated in one reaction, heating and condensing reflux, has created the sodium formate acidification reaction space of optimizing jointly, the while compact conformation, and floor space is little, and equipment investment is few;
(2) adopt the membrane wall heating arrangement.This reaction unit adopts the membrane wall heating arrangement of being made up of jointly some heat exchanger tubes and collection case, compares traditional integral chuck heating arrangement, and its heat transfer efficiency is higher, and structural strength is better, and is efficient and reliable;
(3) the energy utilization is more reasonable.Polyphosphoric acid acidifying sodium formate process, system viscosity begins very thickness, and along with reaction is carried out, under the situation of volatilization or the effective condensing reflux of vaporization formic acid, system viscosity can diminish, and flowability improves.If dispose single agitator according to initial viscosity, then excess drive force can appear in the later stage, and agitator necessarily can not well adapt to the later stage system; Otherwise if dispose single agitator according to later stage viscosity, then it can't normally move because of being short of power in the next meeting of thickness system.This device is according to the system viscosity situation of change, and locellus is operated, and has disposed dissimilar agitators, under the situation of optimizing mixing effect, has realized energy-saving and cost-reducing simultaneously;
(4) continuous operation.This stage acidizing reaction unit can realize that through reasonable control device length, dividing plate height, number of chambers, charging rate etc. material exports just completion reaction from entering the mouth to.Compared to intermittent reaction, continuous operation can be cut down the number of intermediate links, and simplifies the operation, and efficient is higher, is suitable for large-scale production.
Description of drawings
Fig. 1 is the structural representation that the utility model is used for formic acid quantity-produced stage acidizing reaction unit.
Fig. 2 is the side view of Fig. 1.
Among the figure: 1, premix feed(raw material)inlet pipe, 2, first member plate, 3, built-in condenser, 3.1, the refrigerant inlet tube, 3.2, refrigerant inlet collection case; 3.3, condensation tube bank, 3.4, refrigerant exit collection case, 3.5, the refrigerant exit pipe, 4, agitator, 5, fixed mount; 6, right end plate, 7, the reactant liquor outlet, 8, heating jacket, 8.1, the heating agent outlet, 8.2, heating agent outlet collection case; 8.3, the false add heat pipe, 8.4, heating agent inlet collection case, 8.5, heating agent inlet header, 8.6, the heating agent inlet tube, 8.7, heating agent inlet collection case; 9, kettle, 10, dividing plate, 11, upper shell, 12, middle cylinder body, 13, lower shell.
The specific embodiment
Below in conjunction with accompanying drawing and embodiment the utility model is further described.
Shown in Figure 2 like Fig. 1, the utility model comprises the sealing kettle 9 that is surrounded jointly by first member plate 2, right end plate 6, upper shell 11, middle cylinder body 12, lower shell 13; Symmetric arrangement has heating jacket 8 before and after kettle 9 outer lower portion and the outside central region; Kettle 9 inside upper part have hung built-in condenser 3 through fixed mount 5 along axis; The refrigerant inlet tube 3.1 of built-in condenser 3 is drawn through the top of first member plate 2 and right end plate 6 respectively with refrigerant exit pipe 3.5; Premix feed(raw material)inlet pipe 1 is arranged in first member plate 2 bottoms, and the reactant liquor outlet 7 of kettle 9 right-hand member bottoms passes heating jacket 8 from kettle 9 and draws.
Described kettle 9 is divided into a plurality of reative cells by dividing plate 10; All according to the different agitator 4 of the different configurations of regional viscosity of the system that becomes sticky, wherein the initial reaction stage material viscosity is bigger for dividing plate quantity, spacing, adjustable height, each reative cell; Configurable big blade agitators; Along with reaction is carried out, material is thinning, can corresponding configuration vanelets agitator.
Described built-in condenser 3 is one another in series by refrigerant inlet tube 3.1, refrigerant inlet collection case 3.2, condensation tube bank 3.3, refrigerant exit collection case 3.4 and refrigerant exit pipe 3.5 and is welded, and wherein refrigerant inlet collection case 3.2 and refrigerant exit collection case 3.4 constitute by the anti-corrosion steel pipe that closed at both ends and side have the hole that is used for inserting condensation tube bank 3.3.
Described heating jacket 8 adopts membrane wall structure; By two the heating agent inlet tubes 8.5 in top; 8.6, two heating agents inlet collection casees 8.4; 8.7, a plurality of false add heat pipe 8.3, bottom heating agent outlet collection case 8.2 and heating agent outlet 8.1 be welded jointly, wherein false add heat pipe 8.3 bends according to the external diameter of lower shell 13.
In the utility model course of work; Participate in the kettle 9 of premix raw material pipe 1 entering sealing of reaction through the premix feed(raw material)inlet; Here the system temperature can be controlled at about 100 ℃ through the heating agent in the heating jacket 8; Under the situation that has acidification adjuvant formic acid to exist, polyphosphoric acids and sodium formate can step-reactions simultaneously.Wherein the part formic acid product of volatilization or vaporization is under the effect of the built-in condenser 3 in top, and system is returned in condensation in time.Through behind the some cycles, polyphosphoric acids and sodium formate just export from entering the mouth to and react completely, and the product that is rich in formic acid and sodium dihydrogen phosphate of generation can obtain high dense, high-purity formic acid product again through separated.In the course of reaction, in the heating jacket 8 otherwise open closely go into heating agent, the flow of adjustment heating agent can suit and stable reaction temperature for system provide with temperature.Simultaneously, the built-in condenser 3 in top otherwise open close is gone into refrigerant, to avoid influencing reaction because of the mobile variation of system that formic acid volatilization or vaporization cause.
Claims (4)
1. one kind is used for formic acid quantity-produced stage acidizing reaction unit, it is characterized in that: comprise the sealing kettle (9) that is surrounded jointly by first member plate (2), right end plate (6), upper shell (11), middle cylinder body (12), lower shell (13); Symmetric arrangement has heating jacket (8) before and after kettle (9) outer lower portion and the outside central region; Kettle (9) inside upper part has hung built-in condenser (3) through fixed mount (5) along axis; The refrigerant inlet tube (3.1) of built-in condenser (3) and refrigerant exit pipe (3.5) are drawn through the top of first member plate (2) and right end plate (6) respectively; Premix feed(raw material)inlet pipe (1) is arranged in first member plate (2) bottom, and the reactant liquor outlet (7) of kettle (9) right-hand member bottom passes heating jacket (8) from kettle (9) and draws.
2. a kind of formic acid quantity-produced stage acidizing reaction unit that is used for according to claim 1; It is characterized in that: described kettle (9) is divided into a plurality of reative cells by dividing plate (10); Dividing plate quantity, spacing, adjustable height, each reative cell all dispose different agitators (4) according to the regional viscosity difference of the system that becomes sticky.
3. a kind of formic acid quantity-produced stage acidizing reaction unit that is used for according to claim 1; It is characterized in that: described built-in condenser (3) is one another in series with refrigerant exit pipe (3.5) and is welded by refrigerant inlet tube (3.1), refrigerant inlet collection case (3.2), condensation tube bank (3.3), refrigerant exit collection case (3.4), and wherein refrigerant inlet collection case (3.2) and refrigerant exit collection case (3.4) have by closed at both ends and side and be used for inserting the anti-corrosion steel pipe formation that the hole of (3.3) is restrained in condensation.
4. a kind of formic acid quantity-produced stage acidizing reaction unit that is used for according to claim 1; It is characterized in that: described heating jacket (8) adopts membrane wall structure; By two the heating agent inlet tubes (8.5 in top; 8.6), two heating agents inlet collection case (8.4,8.7), a plurality of false add heat pipe (8.3), bottom heating agent outlet collection case (8.2) and heating agent outlets (8.1) are welded jointly, wherein false add heat pipe (8.3) bends according to the external diameter of lower shell (13).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011202010866U CN202122957U (en) | 2011-06-15 | 2011-06-15 | Multistage acidification reactor for continuous production of formic acid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011202010866U CN202122957U (en) | 2011-06-15 | 2011-06-15 | Multistage acidification reactor for continuous production of formic acid |
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| Publication Number | Publication Date |
|---|---|
| CN202122957U true CN202122957U (en) | 2012-01-25 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2011202010866U Expired - Lifetime CN202122957U (en) | 2011-06-15 | 2011-06-15 | Multistage acidification reactor for continuous production of formic acid |
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| CN (1) | CN202122957U (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102320949A (en) * | 2011-06-15 | 2012-01-18 | 浙江大学 | Multistage acidification reaction device for formic acid continuous production |
| CN107096483A (en) * | 2017-04-28 | 2017-08-29 | 佛山市尚峰高分子科技有限公司 | A kind of reactor for waterborne polyurethane resin |
-
2011
- 2011-06-15 CN CN2011202010866U patent/CN202122957U/en not_active Expired - Lifetime
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102320949A (en) * | 2011-06-15 | 2012-01-18 | 浙江大学 | Multistage acidification reaction device for formic acid continuous production |
| CN102320949B (en) * | 2011-06-15 | 2013-07-31 | 浙江大学 | Multistage acidification reaction device for formic acid continuous production |
| CN107096483A (en) * | 2017-04-28 | 2017-08-29 | 佛山市尚峰高分子科技有限公司 | A kind of reactor for waterborne polyurethane resin |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| AV01 | Patent right actively abandoned |
Granted publication date: 20120125 Effective date of abandoning: 20130731 |
|
| RGAV | Abandon patent right to avoid regrant |