CN106467342B - A kind of mother liquor processing method in Production of pentaerythritol - Google Patents

A kind of mother liquor processing method in Production of pentaerythritol Download PDF

Info

Publication number
CN106467342B
CN106467342B CN201610750114.7A CN201610750114A CN106467342B CN 106467342 B CN106467342 B CN 106467342B CN 201610750114 A CN201610750114 A CN 201610750114A CN 106467342 B CN106467342 B CN 106467342B
Authority
CN
China
Prior art keywords
subsider
mother liquor
slot
production
pentaerythritol
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201610750114.7A
Other languages
Chinese (zh)
Other versions
CN106467342A (en
Inventor
施以军
董德昌
翁自飞
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Anhui Jinhe Industrial Co Ltd
Original Assignee
Anhui Jinhe Industrial Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Anhui Jinhe Industrial Co Ltd filed Critical Anhui Jinhe Industrial Co Ltd
Priority to CN201610750114.7A priority Critical patent/CN106467342B/en
Publication of CN106467342A publication Critical patent/CN106467342A/en
Application granted granted Critical
Publication of CN106467342B publication Critical patent/CN106467342B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00—Multistage treatment of water, waste water or sewage
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/38—Treatment of water, waste water, or sewage by centrifugal separation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F2001/007—Processes including a sedimentation step
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F2001/5218—Crystallization
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
    • C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2301/00—General aspects of water treatment
    • C02F2301/04—Flow arrangements
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2301/00—General aspects of water treatment
    • C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions

Abstract

The present invention relates to the mother liquor processing methods in a kind of Production of pentaerythritol, the following steps are included: 1) centrifuge mother liquor in Production of pentaerythritol, it is delivered to progress substep sedimentation in V1, V2, V3, V4, V5, V6 subsider, V1 and V2 temperature is 65 ~ 70 DEG C, and V3, V4, V5, V6 are respectively 45 ~ 50 DEG C, 35 ~ 40 DEG C, 25 ~ 30 DEG C, 18 ~ 23 DEG C；2) mother liquor is filtered using plate and frame filter press after the sedimentation of afterbody subsider.The present invention has the following advantages: improving the benefit of sedimentation；Mother liquor first heats up to cool down afterwards, and pentaerythrite is enable to crystallize out to greatest extent, and the pentaerythrite content in clear liquid greatly reduces after filtering, promotes formic acid sodium content obvious, good product quality；Pentaerythrite content reduces in clear liquid, improves the yield of pentaerythrite.

Description

A kind of mother liquor processing method in Production of pentaerythritol
Technical field
The invention belongs to chemical production technical field, a kind of be related in Production of pentaerythritol mother liquor processing method.
Background technique
Pentaerythrite is used primarily in coatings industry, can be used to manufacture phthalic resin coating, can make hardness, the light of paint film Pool and durability are improved.It also serves as the raw material of rosin needed for colored paint, varnish and printing ink etc., and can stemness processed Oil, smolderability coating and aeroengine oil etc..The aliphatic ester of pentaerythrite is efficient lubricant and plasticizer for polyvinyl chloride, Its epoxides is then the non-raw material from raw surfactant of production.Pentaerythrite easily forms complex compound with metal, is also washing It washs in agent prescription and is used as water softening agent.In addition, being also used to the production such as medicine, pesticide.Contain four in pentaerythrite molecule A equivalent methylol, the symmetry with height, therefore be often used as polyfunctional compound produces raw material.It is nitrified by it Pentaerythritol tetranitrate (pacifying very much, PETN) can be made, be a kind of high explosives；Esterification can obtain pentaerythritol triacrylate (PETA), it is used as coating.
In Production of pentaerythritol, formaldehyde, acetaldehyde are reacted in the case where sodium hydroxide makees catalyst, reaction knot It is quickly neutralized with acid after beam, obtains the mixed liquor of pentaerythrite, sodium formate and water.By rectifying, evaporation, crystallization, centrifugation, drying Obtain pentaerythrite.Being centrifuged workshop section is to separate pentaerythrite with sodium formate, and crude product pentaerythrite and mother liquor are obtained after separation, female Liquid is sent to subsider sedimentation, carried out filtering by plate and frame filter press after sedimentation, pentaerythrite is separated with sodium formate clear liquid.With Toward mother liquor processing method be to be settled using section between single slot, it is not only inefficient, and Ji Wusi in sodium formate clear liquid after filtering Alcohol content is high, leads to high organic content in finished product sodium formate, not only affects sodium formate product quality but also reduce season penta Tetrol yield, while organic matter has seriously affected the stability of system in system circulation.
Summary of the invention:
The object of the invention is in order to overcome in existing mother liquor processing method using present in section sedimentation method between single slot Not only low efficiency, the high determination of pentaerythrite content in sodium formate clear liquid after filtering, in a kind of Production of pentaerythritol provided Mother liquor processing method, substep sedimentation is carried out to mother liquor with continuous high-efficient, and can extract in mother liquor to greatest extent Pentaerythrite reduces the organic matter in sodium formate product, improves sodium formate product quality and pentaerythrite yield.
The purpose of the present invention is what is be achieved by the following technical programs:
A kind of mother liquor processing method in Production of pentaerythritol, comprising the following steps:
1) centrifuge mother liquor in Production of pentaerythritol is delivered in one group of concatenated subsider of at least two and sink step by step Drop, temperature in rear stage subsider are successively decreased a temperature difference than upper level subsider；
2) each subsider is carried out the repeats itself of mother liquor or is delivered in next stage subsider to realize string using circulating pump Connection；
3) mother liquor is filtered using plate and frame filter press after the sedimentation of afterbody subsider；
4) it is respectively equipped with spiral heater and blender in each subsider, heating stirring is carried out to mother liquor.
The subsider can be using containers such as reaction kettle, the tanks industrially used.
Based on the above technical solution, there can be technical solution further below:
One group of subsider is 6, to centrifuge mother liquor using the subsidence style of cooling of successively decreasing afterwards that first heats up, i.e., first Subsider V1 and the second subsider V2 temperature are 65 ~ 70 DEG C, second and third, four, five, six subsider V3, V4, V5, V6 be respectively 45 ~50℃、35~40℃、25~30℃、18~23℃。
Centrifuge mother liquor is first entered into the first subsider V1, then repeats itself and is produced to the second subsider V2, third and fourth, Five, six subsider V3, V4, V5, V6 are repeated in repeats itself and produce the process for arriving next stage subsider, the first subsider V1 Volume is 100m3, second and third, the volume of four, five, six subsider V2, V3, V4, V5, V6 be respectively 60m3。
The blender is divided into upper, middle and lower using three-stage stirrer paddle, and the revolving speed of stirring is 40 ~50r/min。
First subsider V1 circular flow controls 35 ~ 40m3/ h, second and third, four, five, six subsider V2, V3, V4, V5, The circular flow of V6 is respectively 25 ~ 30m3/h。
6 subsiders keep full liquid level, into it is how many go out how many, equipment not ingress of air in slot.
The plate and frame filter press is free flow plate and frame filter press, using continuous uninterrupted filtering.
Mother liquor processing method in Production of pentaerythritol provided by the present invention has the advantage that
1, more previous mother liquor sedimentation, improves the benefit of sedimentation；2, mother liquor first heats up cools down afterwards, the pentaerythrite in mother liquor Recrystallization is achieved the purpose that, so that pentaerythrite is crystallized out to greatest extent, greatly reduced in clear liquid after filtering Pentaerythrite content；3, pentaerythrite is greatly lowered in the filtered clear liquid of mother liquor, promotes formic acid sodium content obvious, formic acid Content of organics reduces in sodium finished product, good product quality；4, pentaerythrite content reduces in clear liquid, and pentaerythrite is in whole system Middle circulation is reduced, and is improved system stability, is improved the yield of pentaerythrite.
Detailed description of the invention:
Fig. 1 is existing Production of pentaerythritol process flow diagram；
Fig. 2 process flow diagram provided by the invention.
Specific implementation method:
Example one:
As shown in Fig. 2, the first subsider V1 is set first, 100 m of volume3, the inside of subsider V1 adds equipped with steam Hot coil and blender, the outside of subsider V1 are equipped with circulating pump, the import connection bottom subsider V1, the outlet point of circulating pump It is not connected to the entrance of end entrance and the second subsider V on subsider V1.Second is set gradually behind the first subsider V1 Subsider V2, third subsider V3, the 4th subsider V4, the 5th subsider V5, the 6th subsider V6, each subsider V2 ... The inside of subsider V6 is equipped with steam(-)coil and blender, and the outside of each subsider V2 ... subsider V5, which is equipped with, to be followed Ring pump, the import of circulating pump connects the same level sedimentation trench bottom, outlet is connected respectively on the same level subsider end entrance and next End entrance is both provided with valve before each entrance certainly on grade subsider.The 6th last bottom subsider V6 connects circulating pump Import, circulating-pump outlet connect plate filter.
The present invention provides the mother liquor processing method in a kind of Production of pentaerythritol, and basic process steps are as follows: 1) will be The mother liquor that system comes opens heating steam and improves temperature, open circulating pump and stirring, adjustment are stirred according to subsider V1 is continuously pumped into It is certain to mix revolving speed；2) internal circulating load and produced quantity are adjusted, keeping subsider V1 liquid level is that full liquid is constant；3) control produced quantity is constant, Subsider V2 is produced, the pump circulation of V2 slot is opened simultaneously and is stirred and heating steam, is controlled certain temperature-resistant；4) from Subsider V2 extraction opens simultaneously the pump circulation and stirring and cooling water of V3 slot to V3 slot, controls certain temperature-resistant；5) Similarly, the operation of V4, V5 and V3 slot is consistent, is finally continuously pumped into plate and frame filter press from V6 slot and is filtered, and obtains pentaerythrite filter Cake and sodium formate clear liquid.
Specific practical operation is as follows: the mother liquor that system is come, according to flow 10m3/ h enters V1 slot, opens the heating of V1 slot and steams Vapour opens the stirring of V1 slot controlled at 65 ~ 70 DEG C, and adjustment speed of agitator is 40 ~ 50r/min, opens circulating pump, adjustment circulation Flow is 35 ~ 40m3/ h, extraction to V2 slot control flow is 10m3/ h controls V1 tank liquor invariant position；After producing mother liquor to V2 slot, Controlled at 65 ~ 70 DEG C, the stirring of V2 slot is opened, adjustment speed of agitator is 40 ~ 50r/min, opens circulating pump, adjusts recycle stream Amount is 25 ~ 30m3/ h, extraction to V3 slot control flow is 10m3/ h controls V2 tank liquor invariant position；After producing mother liquor to V3 slot, control Temperature processed is 45 ~ 50 DEG C, opens the stirring of V3 slot, and adjustment speed of agitator is 40 ~ 50r/min, opens circulating pump, adjusts circular flow For 25 ~ 30m3/ h, extraction to V4 slot control flow is 10m3/ h controls V3 tank liquor invariant position；Similarly V4, V5 slot is as V3 slot, The control of V4 bath temperature degree is 35 ~ 40 DEG C, and the control of V5 bath temperature degree is 25 ~ 30 DEG C；V6 slot is filtered controlled at 18 DEG C, filtering Pentaerythrite content is 9.78% in the clear liquid obtained afterwards, and formic acid sodium content is 33.17%.
Example two:
The mother liquor that system is come, according to flow 10m3/ h carries out V1 slot, and opening V1 slot heating automatic steam control temperature is 65 ~ 70 DEG C, the stirring of V1 slot is opened, adjustment speed of agitator is 40 ~ 50r/min, opens circulating pump, and adjustment circular flow is 35 ~ 40m3/ h, Producing V2 slot control flow is 10m3/ h controls V1 tank liquor invariant position；After producing mother liquor to V2 slot, controlled at 65 ~ 70 DEG C, the stirring of V2 slot is opened, adjustment speed of agitator is 40 ~ 50r/min, opens circulating pump, and adjustment circular flow is 25 ~ 30m3/ h, Producing V3 slot control flow is 10m3/ h controls V2 tank liquor invariant position；After producing mother liquor to V3 slot, controlled at 45 ~ 50 DEG C, the stirring of V3 slot is opened, adjustment speed of agitator is 40 ~ 50r/min, opens circulating pump, and adjustment circular flow is 25 ~ 30m3/ h, Producing V4 slot control flow is 10m3/ h controls V3 tank liquor invariant position；Similarly V4, V5 slot are as V3 slot, V4 bath temperature degree control 35 ~ 40 DEG C are made as, the control of V5 bath temperature degree is 25 ~ 30 DEG C；V6 slot is filtered controlled at 20 DEG C, and what is obtained after filtering is clear Pentaerythrite content is 11.08% in liquid, and formic acid sodium content is 31.87%.
Example three:
The mother liquor that system is come, according to flow 10m3/ h carries out V1 slot, and opening V1 slot heating automatic steam control temperature is 65 ~ 70 DEG C, the stirring of V1 slot is opened, adjustment speed of agitator is 40 ~ 50r/min, opens circulating pump, and adjustment circular flow is 35 ~ 40m3/ h, Producing V2 slot control flow is 10m3/ h controls V1 tank liquor invariant position；After producing mother liquor to V2 slot, controlled at 65 ~ 70 DEG C, the stirring of V2 slot is opened, adjustment speed of agitator is 40 ~ 50r/min, opens circulating pump, and adjustment circular flow is 25 ~ 30m3/ h, Producing V3 slot control flow is 10m3/ h controls V2 tank liquor invariant position；After producing mother liquor to V3 slot, controlled at 45 ~ 50 DEG C, the stirring of V3 slot is opened, adjustment speed of agitator is 40 ~ 50r/min, opens circulating pump, and adjustment circular flow is 25 ~ 30m3/ h, Producing V4 slot control flow is 10m3/ h controls V3 tank liquor invariant position；Similarly V4, V5 slot are as V3 slot, V4 bath temperature degree control 35 ~ 40 DEG C are made as, the control of V5 bath temperature degree is 25 ~ 30 DEG C；V6 slot is filtered controlled at 23 DEG C, and what is obtained after filtering is clear Pentaerythrite content is 12.91% in liquid, and formic acid sodium content is 30.04%.
The above described is only a preferred embodiment of the present invention, being not intended to limit the present invention in any form；Appoint What those skilled in the art, without departing from the scope of the technical proposal of the invention, all using the side of the disclosure above Method and technology contents make many possible changes and modifications to technical solution of the present invention, or are revised as the equivalent reality of equivalent variations Apply example.Therefore, anything that does not depart from the technical scheme of the invention according to the technical essence of the invention do above embodiments Any simple modification, equivalent replacement, equivalence changes and modification, all of which are still within the scope of protection of the technical scheme of the invention.

Claims (3)

1. the mother liquor processing method in a kind of Production of pentaerythritol, it is characterised in that:
1) centrifuge mother liquor in Production of pentaerythritol is delivered to progress substep sedimentation in 6 concatenated subsiders；
2) each subsider is carried out the repeats itself of mother liquor and is delivered in next stage subsider to realize series connection using circulating pump；
3) mother liquor is filtered using plate and frame filter press after the sedimentation of afterbody subsider；
4) it is respectively equipped with spiral heater and blender in each subsider, heating stirring is carried out to mother liquor；
To centrifuge mother liquor using the subsidence style of cooling of successively decreasing afterwards that first heat up, i.e. the first subsider and the second subsider temperature are 65 ~ 70 DEG C, second and third, the temperature of four, five, six subsiders be respectively 45 ~ 50 DEG C, 35 ~ 40 DEG C, 25 ~ 30 DEG C, 18 ~ 23 DEG C；
Centrifuge mother liquor is first entered into the first subsider, then repeats itself and is produced to the second subsider, third and fourth, five, six sedimentations Slot is repeated in repeats itself and produces the process for arriving next stage subsider, and the first sedimentation sump volume is 100m3, second and third, Four, the volume of five, six subsiders is respectively 60m3；
First subsider circular flow controls 35 ~ 40m3/ h, second and third, the circular flows of four, five, six subsiders be respectively 25 ~ 30m3/h；
6 subsiders keep full liquid levels, into it is how many go out how many, equipment not ingress of air in slot.
2. the mother liquor processing method in a kind of Production of pentaerythritol according to claim 1, which is characterized in that the stirring Device is divided into upper, middle and lower using three-stage stirrer paddle, and the revolving speed of stirring is 40 ~ 50r/min.
3. the mother liquor processing method in a kind of Production of pentaerythritol according to claim 1, which is characterized in that the sheet frame pressure Filter is free flow plate and frame filter press, using continuous uninterrupted filtering.
CN201610750114.7A 2016-08-30 2016-08-30 A kind of mother liquor processing method in Production of pentaerythritol Active CN106467342B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610750114.7A CN106467342B (en) 2016-08-30 2016-08-30 A kind of mother liquor processing method in Production of pentaerythritol

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610750114.7A CN106467342B (en) 2016-08-30 2016-08-30 A kind of mother liquor processing method in Production of pentaerythritol

Publications (2)

Publication Number Publication Date
CN106467342A CN106467342A (en) 2017-03-01
CN106467342B true CN106467342B (en) 2019-09-03

Family

ID=58230650

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610750114.7A Active CN106467342B (en) 2016-08-30 2016-08-30 A kind of mother liquor processing method in Production of pentaerythritol

Country Status (1)

Country Link
CN (1) CN106467342B (en)

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1254702A (en) * 1998-11-21 2000-05-31 衡阳三化实业股份有限公司 Process for recovering pentaerythritol and protan from mother liquid of pentaerythritol
CN103570522A (en) * 2013-11-01 2014-02-12 安徽金禾实业股份有限公司 Method for producing 99.5% of sodium formate

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7771681B2 (en) * 2006-12-29 2010-08-10 Nalco Company Method for improved aluminum hydroxide production

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1254702A (en) * 1998-11-21 2000-05-31 衡阳三化实业股份有限公司 Process for recovering pentaerythritol and protan from mother liquid of pentaerythritol
CN103570522A (en) * 2013-11-01 2014-02-12 安徽金禾实业股份有限公司 Method for producing 99.5% of sodium formate

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
"PET晶体生长的影响因素研究";苏佳乐;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20160315(第3期);第B014-1081页

Also Published As

Publication number Publication date
CN106467342A (en) 2017-03-01

Similar Documents

Publication Publication Date Title
SE531608C2 (en) Methods for manufacturing pentaerythritol
CN107935846A (en) A kind of apparatus and method of continuous production environment-friendlyplasticizer plasticizer
CN101223288A (en) Improvements in a process for rapid acid hydrolysis of lignocellulosic material and in a hydrolysis reactor
CN1639184A (en) Process of extracting and purifying phytosterols and phytostanols from tall oil pitch
CN102304094A (en) Preparation method of sulfadoxine and intermediate thereof
CN104910059B (en) The recovery method of cumyl peroxide DCP device circulating mother liquor
CN107986952A (en) A kind of continuous crystallisation process of purifying vanillin
CN113292429B (en) Production system and production method of isobutyl acetate for high-end paint
CN107602373A (en) A kind of method that sodium acetate is extracted from furfural production waste water
CN106699831A (en) Method of preparing liquid crystal cholesterol by using wool fat by virtue of complexing method
CN106467342B (en) A kind of mother liquor processing method in Production of pentaerythritol
CN102329196B (en) Method for separating out mono-pentaerythritol and dipentaerythritol
CN105367425A (en) Purification system for chemical method for preparing BHET monomer from waste PET material
CN105503573B (en) Method and device for separation treatment of sodium formate in NPG (neopentyl glycol) production technology
CN102746134A (en) Method for decreasing content of sodium chloride impurities in recovered sodium formate
CN110194715A (en) A kind of production method of sodium formate
CN109232158A (en) Durol continuous crystallisation process
CN103396309A (en) Method for producing high-purity propylgallate by virtue of pressurization process
CN205616574U (en) Use coking desulfurization waste liquid to carry device of salt extraction filter residue as raw materials purification sodium hyposulfite
CN101863744B (en) Method for separating dichlorophenol mixture by cross-current dissociation extraction
CN111056938A (en) Purification method and purification device for pentaerythritol byproduct crude sodium formate
CN103922925A (en) Production technology of Fenofibric acid
CN1970529A (en) Cardiovascular drug acebutolol intermediate 2- acetyl-4-n-butyramidophenol synthesis method
CN1042140C (en) Method and equipment for continuous hydration degum of vegetable oil
CN102746238A (en) Preparation method of pyrimethanil

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant