CN103130670A - Synthetic leather dimethyl formamide (DMF) recycling residue processing technology and synthetic leather DMF recycling residue processing system - Google Patents

Synthetic leather dimethyl formamide (DMF) recycling residue processing technology and synthetic leather DMF recycling residue processing system Download PDF

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CN103130670A
CN103130670A CN2013100014546A CN201310001454A CN103130670A CN 103130670 A CN103130670 A CN 103130670A CN 2013100014546 A CN2013100014546 A CN 2013100014546A CN 201310001454 A CN201310001454 A CN 201310001454A CN 103130670 A CN103130670 A CN 103130670A
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dmf
dry pot
pot
reclaims
raffinate
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CN103130670B (en
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黄小平
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Blue Ocean Bolong Microfiber Co ltd
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NANPING BOSHIDA ENERGY-SAVING TECHNOLOGY Co Ltd
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Abstract

The invention provides a synthetic leather dimethyl formamide (DMF) recycling residue processing technology and a synthetic leather DMF recycling residue processing system. A negative pressure processing environment is provided for DMF residue, a condensation process, a neutralization recycling process and the like are coordinated, 40% of DMF in DMF residual liquid is recycled, and meanwhile the rest residue is processed through forcing stirring and evaporation to form solid-phase residue, and thus a recovery rate of DMF finished products is improved, discharge amount of the residue is also reduced, the synthetic leather DMF recycling residue processing technology is a technology which can save energy, reduce emission and reduce environmental pollution, and more economic benefits are created for enterprises.

Description

Chemical leather DMF reclaims residue treatment technique and system
Technical field
The present invention relates to a kind of synthetic leather waste recovery and utilize the field, refer in particular to a kind of chemical leather DMF and reclaim residue treatment technique and system.
Background technology
Flourish synthetic leather industry is that numerous enterprises has brought unlimited business opportunity, and for synthetic leather manufacturing concern, as dissolution with solvents PU resin with DMF in the manufacturing processed of PU leather, then flood or cover with paint, lacquer, colour wash, etc. in the surface of base cloth and form bass, utilize the solvability of DMF and water in this process, DMF is washed out, therefore produced the waste water in the wet processing manufacturing processed.Be born the initial stage at Synthetic Leather; waste water is not done to reclaim and directly discharging; but the residue that produces in the DMF of synthetic leather enterprise removal process has also caused certain pollution to environment; in recent years; along with the enhancing of the mankind to environmental protection consciousness; environmental administration makes great efforts to administer the pollution problem of synthetic leather industry repeatly in addition; for the dimethylamine that reclaims in overhead water; most of enterprise has obtained effective improvement by the dimethylamine purification system; but the environmental protection company that all transfers to qualification for residue processes, and enterprise does not have ripe treating method at present.My company has researched and developed this DMF residue treatment technology for this reason, and environment protection and the economic benefit that improves enterprise are all had significant meaning.
Summary of the invention
The object of the invention is to overcome defects, provide a kind of chemical leather DMF to reclaim residue treatment technique and system.
The object of the present invention is achieved like this: a kind of chemical leather DMF reclaims residue treatment technique, and it comprises:
A), produce the step that negative pressure is used for DMF raffinate drying;
Better, in steps A, open vacuum pump apparatus and produce negative pressure in dry pot;
Better, produce negative pressure in described steps A to 0.08MPa;
B), the step that the DMF raffinate that enters is stirred and heats;
Better, in step B, start stirrer and open baiting valve the DMF raffinate is entered in dry pot, then open the heat regulation valve and begin dry pot is heated;
Better, be heated to 150 ℃-200 ℃ in step B;
C), collect the gas that the DMF raffinate is subjected to thermal evaporation, it is carried out condensation, and liquid after condensation is added in alkali and after enter the step of DMF retrieving arrangement re-distillation;
Better, in step C, open cold condenser water circle device, the DMF raffinate enters DMF work in-process storage tank after being subjected to the gas of thermal evaporation to become liquid through condenser condenses in dry pot, with in the alkali that arranges in DMF work in-process storage tank and after raffinate enter DMF retrieving arrangement re-distillation;
D), after the DMF raffinate is disposed, stopped heating is to the logical water-cooled step of dried slag;
Better, in step D, after the DMF raffinate is disposed, close heat regulation valve stopped heating, open the cooling tank inlet valve, by water, that dried slag is cooling;
Better, in step D, circulating water is adopted in water cooling;
E), after dried slag is cooling, carry out exhaust until with the environmental stress balance after get rid of the step of dried slag;
Better, in step e, after dried slag is cooling, opens the emptying drain tap and carry out exhaust, until the dry pot internal and external pressure balance, open the dreg-discharging gate of dry pot, the dried slag in dry pot is discharged outside pot;
Better, after being cooled to below 100 ℃, dried slag carries out exhaust in step e.
The present invention also provides a kind of chemical leather DMF to reclaim slag treatment system, and it comprises vaccum processor, vacuum pump apparatus, DMF work in-process storage tank, condenser, cooling tank, coolant circulation pump, dry pot, stirrer, heating unit and reclaims pot; Described vaccum processor connects vacuum pump apparatus, and vacuum pump apparatus connects dry pot, and described heating unit is set in dry pot, and heating unit is connected with the heat regulation valve, and described stirrer output has stirring-head to stretch in dry pot; Described dry pot one tunnel connects described recoverys pot, and is provided with baiting valve between the two, an end of another road connection condenser of dry pot, and the condenser the other end is connected with DMF work in-process tank; Described cooling tank connects dry pot, and is provided with the cooling tank inlet valve between the two; Also be provided with emptying drain tap and dreg-discharging gate on described dry pot;
In said structure, it also comprises the DMF retrieving arrangement, and the DMF retrieving arrangement is connected with DMF work in-process tank, and is provided with the work in-process tank valve between the two;
In said structure, it also comprises coolant circulation pump, and coolant circulation pump is arranged between cooling tank and dry pot;
In said structure, described vacuum pump apparatus comprises at least 2 vacuum pumps, and described vacuum pump apparatus and vaccum processor and condenser, dry pot are connected.
Beneficial effect of the present invention is to utilize the decomposition of DMF under negative pressure, velocity of evaporation than characteristics faster under normal pressure, and need not add any recovery catalyst in whole removal process, utilize high temperature forced evaporation deacidification principle, remaining solid phase slag is transferred to qualification unit and is concentrated burning disposal.Whole technology can reclaim the DMF that contains 40% in the DMF raffinate, simultaneously thereby remaining residue is formed through the action of forced stirring evaporation rate of recovery that the solid phase slag has improved the DMF finished product, also reduced the discharge capacity of residue, be the technology that a Jie Neng ﹑ Jian Pai ﹑ reduces environmental pollution, created more economic benefit to enterprise.
Description of drawings
Below in conjunction with accompanying drawing in detail concrete structure of the present invention is described in detail
Fig. 1 is system architecture schematic diagram of the present invention.
The 1-vaccum processor; The 2-vacuum pump apparatus; 3-DMF work in-process storage tank; The 4-condenser; The 5-cooling tank; The 6-dry pot; The 7-stirrer; 8-reclaims pot; The 9-coolant circulation pump; The 10-DMF retrieving arrangement; 11-heat regulation valve; 31-work in-process tank valve; 56-cooling tank inlet valve; The 86-baiting valve.
Embodiment
By describing technology contents of the present invention, structural attitude in detail, being realized purpose and effect, below in conjunction with embodiment and coordinate accompanying drawing to be explained in detail.
The residue that existing DMF reclaims by analysis after, roughly form and see the following form:
DMF reclaims residue and forms table
Project Content Proterties
Auxiliary agent. ~5% Liquid
DMF ~40% Liquid
Calcium powder, wood powder and polymkeric substance ~55% Solid
In conjunction with above-mentioned analysis, the invention provides a kind of chemical leather DMF and reclaim residue treatment technique, it comprises:
A), produce the step that negative pressure is used for DMF raffinate drying;
This step is utilized the faster characteristics of the decomposition rate of the higher DMF of temperature, when negative pressure, and the DMF boiling point lowering, the needed heat of decomposing D MF reduces, and service temperature is low, and decomposition rate slows down, energy efficient.
Better, in this step, the negative pressure of DMF raffinate dry environment should be higher than 0.08MPa, and the DMF boiling point is low under this negative pressure, and service temperature is suitable, can reach maximum energy consumption saving.
B), the step that the DMF raffinate that enters is stirred and heats;
Because the boiling point of DMF is 153 ℃, therefore better, the heating to the DMF raffinate in this finally makes service temperature at 150 ℃-200 ℃.By strong stirring, make constantly evaporation and the recovery of liquid that contains in the DMF raffinate thus, the Gu Xing Wu ﹑ Mu Zhi Fen ﹑ Bu Mao ﹑ Tanization Gai ﹑ part small molecules PU ﹑ Zhu Ji ﹑ carbide that stays and polymkeric substance etc. at high temperature stir evaporate to dryness.
C), collect the gas that the DMF raffinate is subjected to thermal evaporation, it is carried out condensation, and liquid after condensation is delivered to the step of DMF retrieving arrangement;
D), after the DMF raffinate evaporates, stopped heating is to the logical water-cooled step of dried slag;
E), after dried slag is cooling, carry out exhaust until with the environmental stress balance after get rid of the step of dried slag;
Best, after being cooled to below 100 ℃, dried slag carries out exhaust in this step.
The technical process of this residue treatment, following turns waste into wealth, and reduces secondary pollution, and existing obvious social benefit has again the principle of economic benefit preferably.Utilize the decomposition of DMF under negative pressure, velocity of evaporation than characteristics faster under normal pressure, when negative pressure, the DMF boiling point lowering, service temperature is low, and the needed heat of decomposing D MF reduces, energy efficient.Need not add any recovery catalyst in whole removal process, utilize high temperature forced evaporation deacidification principle, remaining solid phase slag is transferred to qualification unit and is concentrated burning disposal.Whole technique can reclaim the DMF that contains 40% in the DMF raffinate, simultaneously remaining residue is evaporated the rate of recovery that forms solid phase slag (solid phase 50%, liquid phase 10%) thereby improved the DMF finished product through action of forced stirring, also reduced the discharge capacity of residue, be the technology that a Jie Neng ﹑ Jian Pai ﹑ reduces environmental pollution, created more economic benefit to enterprise.
As Fig. 1, the present invention also provides a kind of chemical leather DMF to reclaim slag treatment system, and it comprises vaccum processor 1, vacuum pump apparatus 2, DMF work in-process storage tank 3, condenser 4, cooling tank 5, dry pot 6, stirrer 7, heating unit and reclaims pot 8.
In above-mentioned, vaccum processor 1 connects vacuum pump apparatus 2, and vacuum pump apparatus 2 connects dry pots 6, and dry pot 6 is interior arranges described heating unit, and heating unit is connected with heat regulation valve 11.7 outputs of described stirrer have stirring-head to stretch in dry pot 6, and dry pot 6 one tunnel connects described recovery pot 8, and are provided with baiting valve 86 between the two, an end of dry pot 6 another roads connection condensers 4, and condenser 4 the other ends are connected with DMF work in-process tank 3; Described cooling tank 5 connects dry pot 6, and is provided with cooling tank inlet valve 56 between the two; Also be provided with emptying drain tap and dreg-discharging gate on described dry pot 6.
As an embodiment, best system also comprises DMF retrieving arrangement 10, and DMF retrieving arrangement 10 is connected with DMF work in-process tank 3, and is provided with work in-process tank valve 31 between the two.
As an embodiment, best system also comprises coolant circulation pump 9, and coolant circulation pump 9 is arranged between cooling tank 5 and dry pot 6;
As an embodiment, better vacuum pump apparatus comprises at least 2 vacuum pumps, and vacuum pump apparatus and vaccum processor 1 and condenser 4, dry pot 6 are connected, and the quantity of vacuum pump is according to the required rank of negative pressure and the situation configuration quantity of coupling device of reaching.
Embodiment:
After chemical leather DMF reclaims, slag treatment system comprises equipment list (vertical)
Figure BDA00002700807600051
The Processing Example of coupling system, technique:
A), open vacuum pump apparatus produce negative pressure in dry pot, negative pressure is to 0.08MPa, and is dry in order to the DMF raffinate;
B), start stirrer and open baiting valve the DMF raffinate is entered in dry pot, then opens the heat regulation valve and begin the dry pot heating, and the red-tape operati temperature is at 150 ℃-200 ℃;
C), open cold condenser water circle device, the DMF raffinate enters DMF work in-process storage tank after being subjected to the gas of thermal evaporation to become liquid through condenser condenses in dry pot, with in the alkali that arranges in DMF work in-process storage tank and after raffinate enter DMF retrieving arrangement re-distillation;
D), after the DMF raffinate evaporates, close heat regulation valve stopped heating, open the cooling tank inlet valve, adopt recirculated water that dried slag is cooling;
E), after dried slag is cooled to 100 ℃, the emptying drain tap of opening dry pot carries out exhaust, until the dry pot internal and external pressure balance, opens the dreg-discharging gate of dry pot, and the dried slag in dry pot is discharged outside pot.
The effect that technical scheme provided by the invention is gone into operation is as follows:
Sequence number Project name Unit Quantity
One Industrial scale ? ?
1 Process level of residue T/ day 2
2 Reclaim DMF(content 35%) T/ day 0.7
Two Operation day in year ? 150
Three Main raw material(s), firing rate ? ?
1 Residue T/ 300
2 Bunker coal T/ 53
Four Utility power consumes ? ?
1 Recirculated water (with reclaiming cooling tower) m3/h 20
2 Electricity consumption (opening 150 days by recovery) Kwh/a 64800
3 Working capacity kw 18
Five Three wastes discharge amount ? ?
? Dried slag after processing T/ 195
Six The device gross investment Ten thousand yuan 105
Seven Annual sales revenue (in DMF) Ten thousand yuan 60
Eight Average annual total cost Ten thousand yuan 9.2
Nine The annual profit total value Ten thousand yuan 50
Ten Payback period ? ?
? If consider the handling of saving ? ?
Electricity is by 0.6 yuan/kwh, and coal is 9.2 ten thousand yuan (not containing Abschreibungskosten and labor wage) by 1000 yuan/t, operation total cost; After this device operation, annual approximately 105 tons of the DMF that reclaim calculate by 5700 yuan/t more, and enterprise increases by 600,000 yuan of sales revenue; Save residue dispose approximately 24.15 ten thousand yuan of expense expenditures (the expense expenditure disposed of Fujian synthetic leather enterprise residue is 2300 yuan/t at present, reducing row's residue 105t year, the expense expenditure by minimum 2300 yuan/t).
As fully visible, the environmental benefit of technical scheme provided by the invention is obvious; From Economic and Efficiency Analysis as can be known, enterprise also can obtain economic benefit preferably when obtaining environmental benefit.
The above is only embodiments of the invention; not thereby limit the scope of the claims of the present invention; every equivalent structure or equivalent flow process conversion that utilizes specification sheets of the present invention and accompanying drawing content to do; or directly or indirectly be used in other relevant technical fields, all in like manner be included in scope of patent protection of the present invention.

Claims (10)

1. a chemical leather DMF reclaims residue treatment technique, it is characterized in that: it comprises,
A), produce the step that negative pressure is used for DMF raffinate drying;
B), the step that the DMF raffinate that enters is stirred and heats;
C), collect the gas that the DMF raffinate is subjected to thermal evaporation, it is carried out condensation, and liquid after condensation is delivered to the step of DMF retrieving arrangement;
D), treat that the DMF raffinate evaporates, stopped heating is to the logical water-cooled step of dried slag;
E), after dried slag is cooling, carry out exhaust until with the environmental stress balance after get rid of the step of dried slag.
2. chemical leather DMF as claimed in claim 1 reclaims residue treatment technique, it is characterized in that:
In described steps A, open vacuum pump apparatus and produce negative pressure in dry pot;
In described step B, start stirrer and open baiting valve the DMF raffinate is entered in dry pot, then open the heat regulation valve and begin dry pot is heated;
In described step C, open cold condenser water circle device, the DMF raffinate enters DMF work in-process storage tank after being subjected to the gas of thermal evaporation to become liquid through condenser condenses in dry pot, with in the alkali that arranges in DMF work in-process storage tank and after raffinate deliver to the DMF retrieving arrangement and again evaporate;
In described step D, after the DMF raffinate evaporates, close heat regulation valve stopped heating, open the cooling tank inlet valve, by water coolant, that dried slag is cooling;
In described step e, after dried slag is cooling, opens the emptying drain tap and carry out exhaust, until the dry pot internal and external pressure balance, open the dreg-discharging gate of dry pot, the dried slag in dry pot is discharged outside pot.
3. chemical leather DMF as claimed in claim 1 or 2 reclaims residue treatment technique, it is characterized in that: produce negative pressure in described steps A to 0.08MPa.
4. chemical leather DMF as claimed in claim 1 or 2 reclaims residue treatment technique, it is characterized in that: be heated to 150 ℃-200 ℃ in described step B.
5. chemical leather DMF as claimed in claim 1 or 2 reclaims residue treatment technique, it is characterized in that: in described step D, circulating water is adopted in water cooling.
6. chemical leather DMF as claimed in claim 1 or 2 reclaims residue treatment technique, it is characterized in that: carry out exhaust in described step e after dried slag is cooled to below 100 ℃.
7. a chemical leather DMF reclaims slag treatment system, it is characterized in that: it comprises vaccum processor, vacuum pump apparatus, DMF work in-process storage tank, condenser, cooling tank, dry pot, stirrer, heating unit and reclaims pot; Described vaccum processor connects vacuum pump apparatus, and vacuum pump apparatus connects dry pot, and described heating unit is set in dry pot, and heating unit is connected with the heat regulation valve, and described stirrer output has stirring-head to stretch in dry pot; Described dry pot one tunnel connects described recoverys pot, and is provided with baiting valve between the two, an end of another road connection condenser of dry pot, and the condenser the other end is connected with DMF work in-process tank; Described cooling tank connects dry pot, and is provided with the cooling tank inlet valve between the two; Also be provided with emptying drain tap and dreg-discharging gate on described dry pot.
8. chemical leather DMF as claimed in claim 7 reclaims slag treatment system, and it is characterized in that: it also comprises the DMF retrieving arrangement, and the DMF retrieving arrangement is connected with DMF work in-process tank, and is provided with the work in-process tank valve between the two.
9. chemical leather DMF as claimed in claim 7 reclaims slag treatment system, and it is characterized in that: it also comprises coolant circulation pump, and coolant circulation pump is arranged between cooling tank and dry pot.
10. chemical leather DMF as claimed in claim 7 reclaims slag treatment system, and it is characterized in that: described vacuum pump apparatus comprises at least 2 vacuum pumps, and described vacuum pump and vaccum processor and condenser, dry pot are connected.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103642513A (en) * 2013-12-03 2014-03-19 浙江工业大学 Method for recycling kettle residues produced after rectification of DMF (dimethyl formamide) from waste obtained by preparation of polyurethane synthetic leather in supercritical/subcritical water
CN104588388A (en) * 2013-10-30 2015-05-06 河北赢丰再生资源利用有限公司 Comprehensive utilization method for chromium-containing leather waste
CN108946850A (en) * 2018-08-14 2018-12-07 河北蓝江生物环保科技有限公司 Evaporate the Retreatment method of raffinate
CN110947733A (en) * 2019-12-04 2020-04-03 浙江旭创环保科技有限公司 Synthetic leather rectification residue recovery process

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104588388A (en) * 2013-10-30 2015-05-06 河北赢丰再生资源利用有限公司 Comprehensive utilization method for chromium-containing leather waste
CN103642513A (en) * 2013-12-03 2014-03-19 浙江工业大学 Method for recycling kettle residues produced after rectification of DMF (dimethyl formamide) from waste obtained by preparation of polyurethane synthetic leather in supercritical/subcritical water
CN103642513B (en) * 2013-12-03 2015-08-26 浙江工业大学 A kind of in super/subcritical water to the recovery and treatment method that the still after the waste material rectifying DMF after preparing Synthetic Leather is residual
CN108946850A (en) * 2018-08-14 2018-12-07 河北蓝江生物环保科技有限公司 Evaporate the Retreatment method of raffinate
CN108946850B (en) * 2018-08-14 2021-07-16 河北蓝江生物环保科技有限公司 Method for reprocessing evaporation raffinate
CN110947733A (en) * 2019-12-04 2020-04-03 浙江旭创环保科技有限公司 Synthetic leather rectification residue recovery process

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