CN109438182A - A kind of production system and its production technology of 99 grades of pentaerythrites - Google Patents
A kind of production system and its production technology of 99 grades of pentaerythrites Download PDFInfo
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- CN109438182A CN109438182A CN201811622120.XA CN201811622120A CN109438182A CN 109438182 A CN109438182 A CN 109438182A CN 201811622120 A CN201811622120 A CN 201811622120A CN 109438182 A CN109438182 A CN 109438182A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/36—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring increasing the number of carbon atoms by reactions with formation of hydroxy groups, which may occur via intermediates being derivatives of hydroxy, e.g. O-metal
- C07C29/38—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring increasing the number of carbon atoms by reactions with formation of hydroxy groups, which may occur via intermediates being derivatives of hydroxy, e.g. O-metal by reaction with aldehydes or ketones
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/78—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by condensation or crystallisation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
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Abstract
The invention discloses the production systems and its production technology of a kind of 99 grades of pentaerythrites, and production system includes the unit that feeds intake set gradually, reaction member, full gear unit, dealcoholysis unit, evaporation element, crystalline element, centrifugal unit and drying unit；The present invention produces pentaerythrite using sodium method continous way, pentaerythrite is using formaldehyde, acetaldehyde as raw material condensation reaction under liquid alkaline catalysis, the stopping of reaction is neutralized with formic acid, pentaerythrite and byproduct formic acid sodium are generated, then obtains 99 grades of pentaerythrite finished products through processes such as full gear, dealcoholysis, evaporation, crystallization and separation dryings.The present invention can be realized single double tripentaerythritol co-production technologies and can reduce the generation of by-product, to improve purity and yield, full gear makes the removal efficiency of formaldehyde reach 99.9%, reduces formaldehyde amount remaining in product.Its degree of automation is higher, and labor intensity and densely populated place degree are all smaller, while also improving the production efficiency of pentaerythrite, reduces the investment of production cost.
Description
Technical field
The invention belongs to the technical field of producing of pentaerythrite, particularly relate to 99 grades of pentaerythrites of one kind
Production system and its production technology.
Background technique
Pentaerythrite, molecular formula C5H12O4, white crystals or powder are flammable, easily by general esterifying organic acid, are largely used to
Coatings industry produces alkyd resin, synthesis quality lubricant, plasticizer, surfactant and the original as medicine, explosive etc.
Material.Pentaerythrite is used primarily in coatings industry, can be used for manufacturing phthalic resin coating, can make the hardness of paint film, gloss and
Durability is improved.The raw material of rosin needed for it also serves as colored paint, varnish and printing ink etc., and can drying oil processed,
Smolderability coating and aeroengine oil etc..The aliphatic ester of pentaerythrite is efficient lubricant and plasticizer for polyvinyl chloride,
Epoxides is then the raw material for producing nonionic surface active agent.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 can be made, be a kind of high explosives；Esterification can obtain pentaerythritol triacrylate, be used as coating.
Furthermore pentaerythrite is also used as the fire retardant of adhesive, expansion type flame retardant can be obtained with ammonium polyphosphate cooperation；It also is used as
The crosslinking agent of polyurethane provides the branch in polyurethane.
Currently, mainly passing through condensation reaction principle when domestic production pentaerythrite, condensing agent is made with sodium hydroxide, is reacted
Formula is 4CH2O+CH3CHO+NaOH=C(CH2OH)4+ HCOONa, in addition to generate pentaerythrite while also generate dipentaerythritol,
Tripentaerythritol, more pentaerythrites, pentaerythrite cyclic formals, sodium formate and micro methanol, are commonly used in the prior art
This technique the shortcomings that be exactly that material proportion fluctuation is big, by-product is more and pentaerythrite contains during the feeding intake of condensation reaction
It measures low.Foreign countries takes continuity method to produce, superior product quality, and energy consumption is lower.The country uses continuous production mode except Yuntianhua,
It can directly produce outside 98 grades, other enterprises are clearance-type condensation process, and 98 grades of products must be made through secondary purification, energy consumption phase
To higher.In addition, domestic pentaerythrite and external speciality produce in application fields such as surfactant, antioxidant, medicine, explosives
Condition ratio still has deficiency, can't substitute.
A kind of preparation of 95 grades of pentaerythrites is disclosed in the patent application document application No. is 201410501653.8
Method, main includes the basic steps such as condensation, preheating, full gear separation and triple effect evaporation, further comprising the steps of: triple effect is steamed
Mixed liquor obtained by hair device is heated；It is centrifuged after mixed liquor is cooled to 80 DEG C~90 DEG C, obtains 95 grades of Ji Wusi by drying
Alcohol；92 grades of pentaerythrites are obtained after mother liquor heating is cooled down again.The 95 grades of pentaerythrite systems provided in above-mentioned patent application document
Although standby method has the characteristics that small investment, low energy consumption, method is simple and product with stable quality.But in preparation season penta
The purity of pentaerythrite can be caused to reduce, acetal content height with the generation of other a large amount of by-products when tetrol；Moreover, making
The degree of automation when standby pentaerythrite is lower, and labor intensity and densely populated place degree are bigger, this preparation in the patent
Method not only reduces the production efficiency of pentaerythrite, while also increasing the investment of production cost.
Summary of the invention
The present invention is in order to overcome the shortcomings of the prior art, the problem of for above-mentioned background technique, provides one
The production system and its production technology of 99 grades of pentaerythrites of kind.
The present invention is achieved by the following technical solutions: a kind of production system of 99 grades of pentaerythrites, the production system
Including the unit that feeds intake, reaction member, full gear unit, dealcoholysis unit, evaporation element, the crystalline element, centrifugal unit set gradually
And drying unit；
The unit that feeds intake includes dilute formaldehyde slot, dilute formaldehyde pump, concentrated formaldehyde slot, concentrated formaldehyde pump, liquid alkaline slot, liquid alkaline pump, acetaldehyde slot, acetaldehyde
Pump, technique sink and technique water pump；Dilute formaldehyde+concentrated formaldehyde is configured to bottom water, and bottom water is the same as water-reducible liquid alkaline and water-reducible second
Aldehyde is together into condensation kettle.
Reaction member includes the first order reaction kettle being sequentially connected in series, first order reaction kettle discharging pump, second order reaction kettle, second order reaction
Kettle discharging pump, third-order reaction kettle, third-order reaction kettle discharging pump, fourth-order reaction kettle, fourth-order reaction kettle discharging pump, neutralization chamber, neutralization
Slot discharging pump and condensation liquid bath；
Four reaction kettle series connection, are on the one hand the reduction of back-mixing degree, on the other hand due to chemical reaction mechanism, need
Different phase reaction temperature is controlled, to meet the production requirement of product.And the temperature of single material in reactor is basic
On be consistent, carried out using multiple reaction kettle connected in series, different reaction kettles can accurately control the reaction temperature in each stage
Degree.
Meanwhile multiple reaction kettle series connection, it can approximately be considered a piston flow reactor, turn under identical operating condition
Rate is also achieved than the high conversion rate of one-pot reaction device so four reaction kettle series connection not only increase the conversion ratio of reaction
Produce serialization.
Full gear unit includes the dealdehyder tower feed pump being sequentially connected in series, condensation liquid preheating tubulation, dealdehyder tower；
Dealcoholysis unit includes the dilute formaldehyde slot of alcohol-containing, dealcoholysis tower feed pump, dealcoholysis tower and the methanol slot being sequentially connected in series；
Evaporation element include the flash vessel being sequentially connected in series, condenser, vacuum pump group, level-one evaporation discharging pump, atmospheric evaporation device and
Dual evaporation discharging pump；
Crystalline element includes the cooled OSLO crystallizer being sequentially connected in series, crystallization discharging pump and centrifugation medial launder；
Cooled OSLO crystallizer is to reach specific degree of supersaturation to saturation feed liquid cooling by external cooler, then by hanging down
Straight pipeline, which enters suspension bed, makes crystal growth, and the biggish particle of volume can contact faster oversaturated solution so can grow
Faster, along with the grading of special crystallisation chamber acts on, the crystal that OSLO crystallizer is produced all have crystal volume it is big,
Grain narrow distribution and uniform feature, while can operate continuously and reduce labor intensity.
Centrifugal unit includes the centrifugation feed pump and belt vacuum filter being sequentially connected in series；
Drying unit includes pan dryer.
It is improved on the basis of old-fashioned pan dryer, increases bottom coohng disk, realized dry and cooling
Integration has prevented the possibility of the exceeded and material moisture condensation of moisture content, while having laid the foundation for subsequent continuous automatic packaging.
The invention also discloses a kind of production technologies of 99 grades of pentaerythrites, specifically comprise the following steps:
S1: the level Four that formaldehyde, acetaldehyde and liquid alkaline are put into reaction member is connected by the unit that feeds intake and is carried out in tank reactor
Condensation reaction obtains mixed component；Mixed component, which is flow to, to be neutralized in kettle and is adjusted to suitable pH with formic acid, and condensation liquid is obtained；
Charge ratio and temperature are automatically controlled by DCS system；
S2: condensation liquid is passed through into preheating step, using the dilute formaldehyde of alcohol-containing as heat source in warm, then by the condensation after preheating
Liquid is delivered to the dealdehyder tower in full gear unit, removes most formaldehyde (removal efficiency is 99.4~99.9%) and 52 in condensation liquid
Pentaerythrite vacuum evaporator is sent into after~57% water；The dilute formaldehyde of alcohol-containing isolates methanol and dilute formaldehyde by dealcoholysis tower, dilute
Formaldehyde feeds intake reuse；
S3: carrying out vacuum flash to pentaerythrite obtained in S2 by evaporation element, will be from the tower reactor of dealdehyder tower resulting season
Penta tetrol mixed liquor is evaporated to 88~94 DEG C, evaporates using atmospheric evaporation device, using the tower top secondary steam of dealdehyder tower as heat
Source, the final liquor ratio weight that evaporates is 1.3；
S4: evaporation liquid is delivered to the cooled OSLO crystallizer in crystalline element, after Continuous Cooling Crystallization, crystal solution be transferred to from
Heart medial launder；
S5: crystal solution is by the belt vacuum filter continuous centrifugal in centrifugal unit, and centrifugation material is using the disk in drying unit
Formula drier is continuous drying to get 99 grades of pentaerythrite finished products.
Preferably, in step S1: the molar concentration of liquid alkaline is 20%, and the molar concentration of formaldehyde is 20%, mole of acetaldehyde
Concentration is 25%.Mixed component is equal in the residence time of first order reaction kettle, second order reaction kettle, third-order reaction kettle and fourth-order reaction kettle
For 30~40min.
Preferably, in step S1: being 6.4-6.8 with the pH that formic acid is adjusted to condensation liquid.First order reaction kettle, second order reaction
The temperature of kettle, third-order reaction kettle and fourth-order reaction kettle is controlled respectively at 22~27 DEG C, 28~33 DEG C, 32~37 DEG C and 38~43
℃.Formaldehyde, acetaldehyde and liquid alkaline are put into reaction member according to the charge ratio that molar ratio is 9.5:1:1.15.
The beneficial effects of the present invention are: the production system and its production technology of 99 grades of pentaerythrites in the present invention use sodium
Method continous way produces pentaerythrite, and pentaerythrite using formaldehyde, acetaldehyde as raw material condensation reaction under liquid alkaline catalysis, stop by reaction midway
Only, and with formic acid it neutralizes, i.e. generation pentaerythrite and byproduct formic acid sodium, then through full gear, dealcoholysis, evaporation, crystallization and separation
The processes such as dry obtain 99 grades of pentaerythrite finished products, and mother liquor goes to steam sodium formate after sedimentation filtration.By by formaldehyde, acetaldehyde with
Liquid alkaline puts into reaction member according to the charge ratio that molar ratio is 9.5:1:1.15, and the present invention can be realized single double tripentaerythritols
Co-production technology and the generation that by-product can be reduced, to improve the purity and yield of resulting 99 grades of pentaerythrites, dealdehyder tower
The removal efficiency of formaldehyde is set to reach 99%.It is used using the dilute formaldehyde of alcohol-containing as heat source, so that the utilization rate of thermal energy increases substantially,
The energy is saved.In addition, the degree of automation of the present invention when producing pentaerythrite is higher, compared with the existing technology in production
Technique, labor intensity and densely populated place degree are all smaller, while also improving the production efficiency of pentaerythrite, reduce production
The investment of cost.Production technology disclosed in the present invention is just able to produce out content using one-step method continuous production and is up to 99%
99 grades of pentaerythrites, and the acetal content for producing pentaerythrite finished product is lower, and therefore, the production of pentaerythrite of the present invention is set
Standby and production technology belongs to advanced level at home.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of 99 grades of Production of pentaerythritol systems of the invention；
Fig. 2 is the process flow chart of 99 grades of Production of pentaerythritol technique of the invention；
In Fig. 1: 1- feeds intake unit；2- reaction member；3- full gear unit；4- dealcoholysis unit；5- evaporation element；6- crystalline element；
7- centrifugal unit；8- drying unit；The dilute formaldehyde slot of 9-；The dilute formaldehyde pump of 10-；11- concentrated formaldehyde slot；12- concentrated formaldehyde pump；13- liquid alkaline
Slot；14- liquid alkaline pump；15- acetaldehyde slot；16- acetaldehyde pump；17- technique sink；18- technique water pump；19- first order reaction kettle；20- mono-
Order reaction kettle discharging pump；21- second order reaction kettle；22- second order reaction kettle discharging pump；23- third-order reaction kettle；24- third-order reaction kettle
Discharging pump；25- fourth-order reaction kettle；26- fourth-order reaction kettle discharging pump；27- neutralization chamber；28- neutralization chamber discharging pump；29- condensation liquid
Slot；30- dealdehyder tower feed pump；31- condensation liquid preheats tubulation；32- dealdehyder tower；The dilute formaldehyde slot of 33- alcohol-containing；The charging of 34- dealcoholysis tower
Pump；35- dealcoholysis tower；36- methanol slot；37- flash vessel；38- condenser；39- vacuum pump group；40- level-one evaporates discharging pump；41-
Atmospheric evaporation device；42- dual evaporation discharging pump；43- cooled OSLO crystallizer；44- crystallizes discharging pump；45- is centrifuged medial launder；
46- is centrifuged feed pump；47- belt vacuum filter；48- pan dryer.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with attached drawing and specific implementation
The present invention is described in detail for example.
Embodiment 1: a kind of production technology of 99 grades of pentaerythrites, the production technology include the following steps:
S1: formaldehyde, acetaldehyde are reacted with liquid alkaline according to the charge ratio investment that molar ratio is 9.5:1:1.15 by feeding intake unit 1
Condensation reaction is carried out in level Four series connection tank reactor in unit 2, obtains mixed component；Wherein first order reaction kettle 19, second level
The temperature of reaction kettle 21, third-order reaction kettle 23 and fourth-order reaction kettle 25 is controlled respectively at 22 DEG C, 28 DEG C, 32 DEG C, 38 DEG C；It is final mixed
It is combined to branch to and neutralizes in kettle and be adjusted to suitable pH with formic acid, obtain condensation liquid；Charge ratio and temperature pass through DCS system
System automatically controls；
S2: using the dilute formaldehyde of alcohol-containing as heat source when condensation liquid is preheated, the condensation liquid after preheating is then delivered to full gear unit 3
In dealdehyder tower 32, be sent into pentaerythrite vacuum evaporator after removing 99.4% formaldehyde and 52% water；The dilute formaldehyde of alcohol-containing passes through de-
Alcohol unit 4 passes through dealcoholysis tower 35, isolates methanol and dilute formaldehyde, and dilute formaldehyde feeds intake reuse；
S3: carrying out vacuum flash to pentaerythrite obtained in S2 by evaporation element 5, will be resulting from the tower reactor of dealdehyder tower 32
Pentaerythrite mixed liquor is evaporated to 88 DEG C, evaporates using atmospheric evaporation device 41, using the tower top secondary steam of dealdehyder tower as heat
Source, the final liquor ratio weight that evaporates is 1.3；
S4: evaporation liquid is delivered to the cooled OSLO crystallizer 43 in crystalline element 6, and after Continuous Cooling Crystallization, crystal solution is transferred to
To centrifugation medial launder 45；
S5: crystal solution is by 47 continuous centrifugal of belt vacuum filter in centrifugal unit 7, and centrifugation material is using in drying unit 8
Pan dryer 48 it is continuous drying to get 99 grades of pentaerythrite finished products.
In S1, mixed component is in first order reaction kettle 19, second order reaction kettle 21, third-order reaction kettle 23 and fourth-order reaction kettle 25
Residence time is 30min；It is 6.4 with the pH that formic acid is adjusted to condensation liquid.
1 result of embodiment: 10m399 crystal solution is centrifuged to obtain 2.74 tons of 99 monopentaerythritol of finished product, single cropping content
99.4%, double season contents 0.1%, acetal content 0.8%, hydroxyl 49.46%, moisture content: 0.04%, ash content: 0.01%, coloration:
40, fusing point: 261 DEG C.
Embodiment 2: a kind of production technology of 99 grades of pentaerythrites, the production technology include the following steps:
S1: formaldehyde, acetaldehyde are reacted with liquid alkaline according to the charge ratio investment that molar ratio is 9.5:1:1.15 by feeding intake unit 1
Condensation reaction is carried out in level Four series connection tank reactor in unit 2, obtains mixed component；Wherein first order reaction kettle 19, second level
The temperature of reaction kettle 21, third-order reaction kettle 23 and fourth-order reaction kettle 25 is controlled respectively at 25 DEG C, 30 DEG C, 35 DEG C, 40 DEG C；It is final mixed
It is combined to branch to and neutralizes in kettle and be adjusted to suitable pH with formic acid, obtain condensation liquid；Charge ratio and temperature pass through DCS system
System automatically controls；
S2: using the dilute formaldehyde of alcohol-containing as heat source when condensation liquid is preheated, the condensation liquid after preheating is then delivered to full gear unit 3
In dealdehyder tower 32, be sent into pentaerythrite vacuum evaporator after removing 99.6% formaldehyde and 54% water, the dilute formaldehyde of alcohol-containing passes through de-
Alcohol unit 4 passes through dealcoholysis tower 35, isolates methanol and dilute formaldehyde, and dilute formaldehyde feeds intake reuse；
S3: carrying out vacuum flash to pentaerythrite obtained in S2 by evaporation element 5, will be from dealdehyder tower 32 tower reactor resulting season
Penta tetrol mixed liquor is evaporated to 90 DEG C, evaporates using atmospheric evaporation device 42, using the tower top secondary steam of dealdehyder tower as heat source,
Final evaporation liquor ratio weight is 1.3；
S4: evaporation liquid is delivered to the cooled OSLO crystallizer 43 in crystalline element 6, and after Continuous Cooling Crystallization, crystal solution is transferred to
To centrifugation medial launder 45；
S5: crystal solution is by 47 continuous centrifugal of belt vacuum filter in centrifugal unit 7, and centrifugation material is using in drying unit 8
Pan dryer 48 it is continuous drying to get 99 grades of pentaerythrite finished products.
In S1, mixed component is in first order reaction kettle 19, second order reaction kettle 21, third-order reaction kettle 23 and fourth-order reaction kettle 25
Residence time is 35min；It is 6.5 with the pH that formic acid is adjusted to condensation liquid.
2 result of embodiment: 10m399 crystal solution is centrifuged to obtain 2.75 tons of 99 monopentaerythritol of finished product, single cropping content
99.5%, double season contents 0.1%, acetal content 0.9%, hydroxyl 49.49%, moisture content: 0.05%, ash content: 0.02%, coloration:
40, fusing point: 261 DEG C.
Embodiment 3: a kind of production technology of 99 grades of pentaerythrites, the production technology include the following steps:
S1: formaldehyde, acetaldehyde are reacted with liquid alkaline according to the charge ratio investment that molar ratio is 9.5:1:1.15 by feeding intake unit 1
Condensation reaction is carried out in level Four series connection tank reactor in unit 2, obtains mixed component；Wherein first order reaction kettle 19, second level
The temperature of reaction kettle 21, third-order reaction kettle 23 and fourth-order reaction kettle 25 is controlled respectively at 26 DEG C, 31 DEG C, 36 DEG C, 41 DEG C；It is final mixed
It is combined to branch to and neutralizes in kettle and be adjusted to suitable pH with formic acid, obtain condensation liquid；Charge ratio and temperature pass through DCS system
System automatically controls；
S2: using the dilute formaldehyde of alcohol-containing as heat source when condensation liquid is preheated, the condensation liquid after preheating is then delivered to full gear unit 3
In dealdehyder tower, be sent into pentaerythrite vacuum evaporator after removing 99.7% formaldehyde and 56% water；The dilute formaldehyde of alcohol-containing passes through dealcoholysis
Unit 4 passes through dealcoholysis tower 35, isolates methanol and dilute formaldehyde, and dilute formaldehyde feeds intake reuse；
S3: carrying out vacuum flash to pentaerythrite obtained in S2 by evaporation element 5, will be from the tower reactor of dealdehyder tower resulting season
Penta tetrol mixed liquor is evaporated to 92 DEG C, evaporates using atmospheric evaporation device 41, using the tower top secondary steam of dealdehyder tower as heat source,
Final evaporation liquor ratio weight is 1.3；
S4: evaporation liquid is delivered to the cooled OSLO crystallizer 43 in crystalline element 6, and after Continuous Cooling Crystallization, crystal solution is transferred to
To centrifugation medial launder 45；
S5: crystal solution is by 47 continuous centrifugal of belt vacuum filter in centrifugal unit 7, and centrifugation material is using in drying unit 8
Pan dryer 48 it is continuous drying to get 99 grades of pentaerythrite finished products.
In S1, mixed component is in first order reaction kettle 19, second order reaction kettle 21, third-order reaction kettle 23 and fourth-order reaction kettle 25
Residence time is 38min；It is 6.7 with the pH that formic acid is adjusted to condensation liquid.
3 result of embodiment: 10m399 crystal solution is centrifuged to obtain 2.76 tons of 99 monopentaerythritol of finished product, single cropping content
99.5%, double season contents 0.1%, acetal content 0.9%, hydroxyl 49.52%, moisture content: 0.03%, ash content: 0.01%, coloration:
40, fusing point: 261 DEG C.
Embodiment 4: a kind of production technology of 99 grades of pentaerythrites, the production technology include the following steps:
S1: formaldehyde, acetaldehyde are reacted with liquid alkaline according to the charge ratio investment that molar ratio is 9.5:1:1.15 by feeding intake unit 1
Condensation reaction is carried out in level Four series connection tank reactor in unit 2, obtains mixed component；Wherein first order reaction kettle 19, second level
The temperature of reaction kettle 21, third-order reaction kettle 23 and fourth-order reaction kettle 25 is controlled respectively at 27 DEG C, 33 DEG C, 37 DEG C, 43 DEG C；It is final mixed
It is combined to branch to and neutralizes in kettle and be adjusted to suitable pH with formic acid, obtain condensation liquid；Charge ratio and temperature pass through DCS system
System automatically controls；
S2: using the dilute formaldehyde of alcohol-containing as heat source when condensation liquid is preheated, the condensation liquid after preheating is then delivered to full gear unit 3
In dealdehyder tower, be sent into pentaerythrite vacuum evaporator after removing 99.9% formaldehyde and 57% water；The dilute formaldehyde of alcohol-containing passes through dealcoholysis
Unit 4 passes through dealcoholysis tower 35, isolates methanol and dilute formaldehyde, and dilute formaldehyde feeds intake reuse；
S3: carrying out vacuum flash to pentaerythrite obtained in S2 by evaporation element 5, will be from the tower reactor of dealdehyder tower resulting season
Penta tetrol mixed liquor is evaporated to 94 DEG C, evaporates using atmospheric evaporation device 43, using the tower top secondary steam of dealdehyder tower as heat source,
Final evaporation liquor ratio weight is 1.3；
S4: evaporation liquid is delivered to the cooled OSLO crystallizer 43 in crystalline element 6, and after Continuous Cooling Crystallization, crystal solution is transferred to
To centrifugation medial launder 45；
S5: crystal solution is by 47 continuous centrifugal of belt vacuum filter in centrifugal unit 7, and centrifugation material is using in drying unit 8
Pan dryer 48 it is continuous drying to get 99 grades of pentaerythrite finished products.
In S1, mixed component is in first order reaction kettle 19, second order reaction kettle 21, third-order reaction kettle 23 and fourth-order reaction kettle 25
Residence time is 40min；Being adjusted to the pH of condensation liquid with formic acid in S1 is 6.8.
4 result of embodiment: 10m399 crystal solution is centrifuged to obtain 2.76 tons of 99 monopentaerythritol of finished product, single cropping content
99.4%, double season contents 0.1%, acetal content 0.8%, hydroxyl 49.56%, moisture content: 0.04%, ash content: 0.02%, coloration:
40, fusing point: 261 DEG C.
Finally it should be noted that the above content is merely illustrative of the technical solution of the present invention, rather than the present invention is protected
The limitation of range, the simple modification or equivalent replacement that those skilled in the art carry out technical solution of the present invention,
All without departing from the spirit and scope of technical solution of the present invention.
Claims (7)
1. a kind of production system of 99 grades of pentaerythrites, it is characterised in that: the production system includes the list that feeds intake set gradually
Member, reaction member, full gear unit, dealcoholysis unit, evaporation element, crystalline element, centrifugal unit and drying unit；
The unit that feeds intake include dilute formaldehyde slot, dilute formaldehyde pump, concentrated formaldehyde slot, concentrated formaldehyde pump, liquid alkaline slot, liquid alkaline pump, acetaldehyde slot,
Acetaldehyde pump, technique sink and technique water pump；
The reaction member includes the first order reaction kettle being sequentially connected in series, first order reaction kettle discharging pump, second order reaction kettle, second order reaction
Kettle discharging pump, third-order reaction kettle, third-order reaction kettle discharging pump, fourth-order reaction kettle, fourth-order reaction kettle discharging pump, neutralization chamber, neutralization
Slot discharging pump and condensation liquid bath；
The full gear unit includes the dealdehyder tower feed pump being sequentially connected in series, condensation liquid preheating tubulation, dealdehyder tower；
The dealcoholysis unit includes the dilute formaldehyde slot of alcohol-containing, dealcoholysis tower feed pump, dealcoholysis tower and the methanol slot being sequentially connected in series；
The evaporation element includes the flash vessel being sequentially connected in series, condenser, vacuum pump group, level-one evaporation discharging pump, atmospheric evaporation
Device and dual evaporation discharging pump；
The crystalline element includes the cooled OSLO crystallizer being sequentially connected in series, crystallization discharging pump and centrifugation medial launder；
The centrifugal unit includes the centrifugation feed pump and belt vacuum filter being sequentially connected in series；
The drying unit includes pan dryer.
2. a kind of production technology of 99 grades of pentaerythrites, it is characterised in that: the production technology specifically comprises the following steps:
S1: the level Four that formaldehyde, acetaldehyde and liquid alkaline are put into reaction member is connected by the unit that feeds intake and is carried out in tank reactor
Condensation reaction obtains mixed component；Mixed component, which is flow to, to be neutralized in kettle and is adjusted to suitable pH with formic acid, and condensation liquid is obtained；
The charge ratio and temperature are automatically controlled by DCS system；
S2: condensation liquid is passed through into preheating step, using the dilute formaldehyde of alcohol-containing as heat source in warm, then by the condensation after preheating
Liquid is delivered to the dealdehyder tower in full gear unit, remove most formaldehyde in condensation liquid and 52~57% water after be sent into Ji Wusi
Alcohol vacuum evaporator；The dilute formaldehyde of alcohol-containing isolates methanol and dilute formaldehyde by dealcoholysis tower, and dilute formaldehyde feeds intake reuse；
S3: carrying out vacuum flash to pentaerythrite obtained in S2 by evaporation element, will be from the tower reactor of dealdehyder tower resulting season
Penta tetrol mixed liquor is evaporated to 88~94 DEG C, evaporates using atmospheric evaporation device, using the tower top secondary steam of dealdehyder tower as heat
Source, the final liquor ratio weight that evaporates is 1.3；
S4: evaporation liquid is delivered to the cooled OSLO crystallizer in crystalline element, after Continuous Cooling Crystallization, crystal solution be transferred to from
Heart medial launder；
S5: crystal solution is by the belt vacuum filter continuous centrifugal in centrifugal unit, and centrifugation material is using the disk in drying unit
Formula drier is continuous drying to get 99 grades of pentaerythrite finished products.
3. a kind of production technology of 99 grades of pentaerythrites according to claim 2, it is characterised in that: in the step S1:
The molar concentration of liquid alkaline is 20%, and the molar concentration of formaldehyde is 20%, and the molar concentration of acetaldehyde is 25%.
4. a kind of production technology of 99 grades of pentaerythrites according to claim 2, it is characterised in that: in the step S1:
Mixed component the residence time of first order reaction kettle, second order reaction kettle, third-order reaction kettle and fourth-order reaction kettle be 30~
40min。
5. a kind of production technology of 99 grades of pentaerythrites according to claim 2, it is characterised in that: in the step S1:
It is 6.4-6.8 with the pH that formic acid is adjusted to condensation liquid.
6. a kind of production technology of 99 grades of pentaerythrites according to claim 2, it is characterised in that: in the step S1:
First order reaction kettle, second order reaction kettle, third-order reaction kettle and fourth-order reaction kettle temperature controlled respectively in 22~27 DEG C, 28~33
DEG C, 32~37 DEG C and 38~43 DEG C.
7. a kind of production technology of 99 grades of pentaerythrites according to claim 2, it is characterised in that: in the step S1:
Formaldehyde, acetaldehyde and liquid alkaline are put into reaction member according to the charge ratio that molar ratio is 9.5:1:1.15.
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| CN114315517A (en) * | 2021-12-31 | 2022-04-12 | 赤峰瑞阳化工有限公司 | Production method of low-energy-consumption 98-grade pentaerythritol |
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Denomination of invention: A production system of 99 grade pentaerythritol and its production process Effective date of registration: 20220422 Granted publication date: 20210427 Pledgee: Chifeng Branch of China Construction Bank Co.,Ltd. Pledgor: CHIFENG RUIYANG CHEMICAL CO.,LTD. Registration number: Y2022150000032 |