CN108680462A - Evaluation method for reaction end in water-soluble thiocarbamide urea formaldehyde building-up process - Google Patents
Evaluation method for reaction end in water-soluble thiocarbamide urea formaldehyde building-up process Download PDFInfo
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- CN108680462A CN108680462A CN201810372030.3A CN201810372030A CN108680462A CN 108680462 A CN108680462 A CN 108680462A CN 201810372030 A CN201810372030 A CN 201810372030A CN 108680462 A CN108680462 A CN 108680462A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The present invention relates to a kind of evaluation methods for reaction end in water-soluble thiocarbamide urea formaldehyde building-up process；Viscosity determinator is installed in reactor, and is allowed to be immersed under the liquid level of reaction solution；Under stirring action of the blender to reaction solution, the variation of on-line determination reaction solution viscosity number；When the viscosity number of solution is between 35.7~40.8mPas, stop reaction, you can obtain water-soluble sulphur urea resin product.The invention avoids continuous samplings, and the method for reaction end is judged using cloud point titration, but by using the viscosity number for measuring reaction solution in reactor, reflect the condensation degree of dissolved of polycondensation product in water-soluble thiocarbamide urea formaldehyde building-up process indirectly, and then has achieved the purpose that in real time, accurately to control reaction end in water-soluble thiocarbamide urea formaldehyde building-up process.
Description
Technical field
The invention belongs to the synthesis technical fields of thiocarbamide urea formaldehyde more particularly to a kind of water-soluble thiocarbamide urea formaldehyde to synthesize
The evaluation method of reaction end in journey.
Background technology
Thiocarbamide urea formaldehyde containing thiourea group has stronger suction-operated to heavy metal, cadmium, lead, chromium etc., therefore
It is widely used in the improvement field of Heavy-metal Polluted Environment.The thiocarbamide urea formaldehyde containing thiourea group is height not soluble in water at present
Molecular organic, therefore its application range primary limitation is in the field of waste water treatment containing heavy metal.Product of the present invention is water-soluble
Thiocarbamide urea formaldehyde containing thiourea group can both give full play to the resinoid cost as a kind of novel heavy metal treatment agent
Low, the simple advantage of synthesis technology, and the application range of this resinoid can be expanded, therefore with before boundless application
Scape.
Macromolecule containing thiourea functional group is a kind of outstanding stabilization agent, is had to heavy metal ion extraordinary
Sequestering power, but trapping agent synthesized at present is solid organic polymer not soluble in water, be can be only applied to in water body
The improvement of heavy metal pollution.
Invention content
Product of the present invention is a kind of newly synthesized water-soluble macromolecule organic containing thiourea group, then both can be abundant
It plays that such chelating resin is at low cost, the simple advantage of synthesis technology, and the application range of this kind of trapping agent can be expanded, have
Boundless foreground.
The building-up process of water-soluble thiocarbamide urea formaldehyde includes mainly two stages of reaction：First stage is addition reaction, is claimed
Be hydroxymethylation.Second stage is polycondensation reaction stage, referred to as methylenation.Water-soluble thiocarbamide urea formaldehyde
Synthesis technology is：By formaldehyde and thiocarbamide with molar ratio for 2.8:1 ratio mixing, at 60 DEG C, reacts under conditions of pH=7.8
30min；80 DEG C are heated to, pH is adjusted to 4.5, the reaction was continued to terminal；PH is adjusted to neutrality, stops heating, is cooled to room
Temperature.Prepare water-soluble thiocarbamide urea formaldehyde.
Methylol chemically reacts：
Methylene chemically reacts：
And the control planning of polycondensation reaction terminal to thiocarbamide urea formaldehyde whether be water-soluble key.In water-soluble thiocarbamide aldehyde
The judgement of resin Experimental room synthesis phase, polycondensation reaction terminal is mainly carried out using cloud point titration, that is, passes through Lentinus Edodes
Method controls the condensation degree of dissolved of the product of polycondensation reaction stage.However, due to sampling and accordingly in plant produced building-up process
Continuous mode need the regular hour, therefore cannot to polycondensation reaction stage realize in real time monitoring, hysteresis quality is apparent, Jin Erwu
Method timely and effectively judges reaction end.If polycondensation reaction ahead of time terminate, condensation degree of dissolved does not reach requirement, properties of product by
It influences；If polycondensation reaction time is long, the condensation degree of dissolved of polycondensation product will be caused excessively high, so that polycondensation reaction is produced
Object generates excessive netted and body shape structure, ultimately generates solid product, and cannot get water-soluble thiocarbamide urea formaldehyde.
It is an object of the invention to overcome the defect of current cloud point titration, provide it is a kind of easy to operate, can in real time, it is accurate
The method for really judging reaction end in water-soluble thiocarbamide urea formaldehyde building-up process.
The present invention's is mainly characterized in that：Due in polycondensation process, increasing with the degree of polymerization of polycondensation product,
Significant change also has occurred in the viscosity of reaction solution.The present invention's the study found that be to ensure that the product of polycondensation reaction is water-soluble
Product, under certain reaction condition, the viscosity number of reaction solution is between 35.7~40.8mPas, the polymerization of polycondensation product
Degree is linear with the viscosity of reaction solution.To sum up, the present invention is by using the viscosity for measuring solution in polycondensation process
Value, to be indirectly controlled polycondensation reaction stage product condensation degree of dissolved, and then in real time, accurately achieve and judge that polycondensation is anti-
Answer the purpose of terminal.
Technical solution of the present invention is as follows：
A kind of evaluation method for reaction end in water-soluble thiocarbamide urea formaldehyde building-up process；When the viscosity number of solution reaches
When to 35.7~40.8mPas, stops reaction, obtain water-soluble sulphur urea resin product.
The present invention installs viscosity determinator in reactor, and is allowed to be immersed under the liquid level of reaction solution；In blender
To under the stirring action of reaction solution, the viscosity number of on-line determination solution.
Because viscosity reflects that the feature of fluid behavior, the concept of viscosity are exactly the concept of interior friction between fluid molecule.
The essence of viscosity is exactly in the fluid flowed, and the flowing velocity size of the cross section upper fluid perpendicular with flow direction is not
Same reason.Since viscosity is one of important physical property of fluid, then, the measurement of viscosity is very heavy in the industrial production
It wants, application range is also very wide.Viscosity is used for the quality and technology controlling and process of finished product in industrial production, due to point of compound
Sub- size, shape directly affect the viscosity of its solution, and because its bulk of molecule, shape and arrangement directly determine the property of its finished product
Matter, so the viscosity of high-molecular compound solution and the property of compound are directly associated.
Main advantages of the present invention are：In the building-up process of water-soluble thiocarbamide urea formaldehyde, the invention avoids continuous
It samples, and judges the method for reaction end using cloud point titration, but by using reaction solution in measurement reactor
Viscosity number, reflects the condensation degree of dissolved of polycondensation product in water-soluble thiocarbamide urea formaldehyde building-up process indirectly, and then has reached real-time
Ground, the purpose for accurately controlling reaction end in water-soluble thiocarbamide urea formaldehyde building-up process.Viscosity is one kind of fluid viscosity
Measurement, is a kind of expression of the fluid flow forces to its internal friction phenomenon.The measurement of viscosity parameter, for predicting production mistake
The operability of technology controlling and process, transporting and the product of journey when in use has important guiding value, in printing, medicine, stone
All conglomeraties such as oil, automobile have great significance.The characteristic of liquid often with other characteristics such as color of product, density, surely
Qualitative, the change of solid component content and molecular weight has relationship, and detects the most convenient of these characteristics and sensitive method is exactly
The viscosity of on-line checking liquid.Online viscosity measurements are carried out according to the range of process specifications in process of production, it can be most
The downtime of the scrappage and production line of the reduction product of limits.
Specific implementation mode
With reference to specific embodiment, the present invention is described further.
Embodiment 1
A method of controlling reaction end in water-soluble thiocarbamide urea formaldehyde building-up process using reaction solution viscosity, by
Following step forms：
(1) viscosity determinator is installed in reactor；
(2) raw material needed for reaction is added in reactor, and viscosity determinator is made to be immersed under liquid level, viscosimetric analysis
Instrument is separately mounted to the position of upper, middle and lower three of reaction vessel, using the average value for the viscosity number that three positions measure respectively,
As final viscosity measurement；
(3) it is 2.5 in the molar ratio of formaldehyde and thiocarbamide:1, the methylolation stage should be in pH=7.5-8.0,60 DEG C of item
30min is reacted under part；Polycondensation reaction stage carries out the conjunction of water-soluble thiocarbamide urea formaldehyde under conditions of pH=4.5-5.0,80 DEG C
At process, under the stirring action of blender, the viscosity number of reaction solution is monitored on-line, when viscosity number is 35.7mPas,
Stop reaction, you can obtain water-soluble sulphur urea resin product.
In the present embodiment, stop product obtained by the reaction when the viscosity number of solution is 35.7mPas, for water-soluble sulphur
Lauxite does not have in product solid precipitation to occur.The experiment that comparison is carried out using cloud point titration, obtained reactor product
In there is solid precipitation, show that polycondensation reaction stage spent time is long, the degree of polymerization of polycondensation product is bigger than normal.
Embodiment 2
A method of controlling reaction end in water-soluble thiocarbamide urea formaldehyde building-up process using reaction solution viscosity, by
Following step forms：
(1) viscosity determinator is installed in reactor；
(2) raw material needed for reaction is added in reactor, and viscosity determinator is made to be immersed under liquid level；
(3) it is 2.5 in the molar ratio of formaldehyde and thiocarbamide:1, the methylolation stage should be in pH=7.5-8.0,60 DEG C of item
30min is reacted under part；Polycondensation reaction stage carries out the conjunction of water-soluble thiocarbamide urea formaldehyde under conditions of pH=4.5-5.0,80 DEG C
At process, under the stirring action of blender, the viscosity number of reaction solution is monitored on-line, when viscosity number is 39.3mPas,
Stop reaction, you can obtain water-soluble sulphur urea resin product.
In the present embodiment, stop product obtained by the reaction when the viscosity number of solution is 39.3mPas, for water-soluble sulphur
Lauxite does not have in product solid precipitation to occur.The experiment that comparison is carried out using cloud point titration, obtained reactor product
In there is solid precipitation, show that polycondensation reaction stage spent time is long, the degree of polymerization of polycondensation product is bigger than normal.
Embodiment 3
A method of controlling reaction end in water-soluble thiocarbamide urea formaldehyde building-up process using reaction solution viscosity, by
Following step forms：
(1) viscosity determinator is installed in reactor；
(2) raw material needed for reaction is added in reactor, and viscosity determinator is made to be immersed under liquid level；
(3) it is 2.5 in the molar ratio of formaldehyde and thiocarbamide:1, the methylolation stage should be in pH=7.5-8.0,60 DEG C of item
30min is reacted under part；Polycondensation reaction stage carries out the conjunction of water-soluble thiocarbamide urea formaldehyde under conditions of pH=4.5-5.0,80 DEG C
At process, under the stirring action of blender, the viscosity number of reaction solution is monitored on-line, when viscosity number is 40.8mPas,
Stop reaction, you can obtain water-soluble sulphur urea resin product.
In the present embodiment, stop product obtained by the reaction when the viscosity number of solution is 40.8mPas, for water-soluble sulphur
Lauxite does not have in product solid precipitation to occur.The experiment that comparison is carried out using cloud point titration, obtained reactor product
In there is solid precipitation, show that polycondensation reaction stage spent time is long, the degree of polymerization of polycondensation product is bigger than normal.
A kind of controlled using reaction solution viscosity proposed by the present invention is reacted in water-soluble thiocarbamide urea formaldehyde building-up process
The method of terminal, is described by embodiment, and related technical personnel can obviously not depart from the content of present invention, spirit and model
It encloses interior changed to the techniques described herein and realizes the present invention with combining.In particular, it should be pointed out that all similar replacements
Apparent to those skilled in the art with changing, they are considered as including in spirit of that invention, range and interior
Rong Zhong.
Claims (2)
1. the evaluation method for reaction end in water-soluble thiocarbamide urea formaldehyde building-up process；It is characterized in that when the viscosity number of solution
When reaching 35.7~40.8mPas, stops reaction, obtain water-soluble sulphur urea resin product.
2. the method as described in claim 1 it is characterized in that installing viscosity determinator in reactor, and is allowed to be immersed in reaction
Under the liquid level of liquid；Under stirring action of the blender to reaction solution, the viscosity number of on-line determination solution.
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| CN201810372030.3A CN108680462A (en) | 2018-04-24 | 2018-04-24 | Evaluation method for reaction end in water-soluble thiocarbamide urea formaldehyde building-up process |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111751248A (en) * | 2020-07-03 | 2020-10-09 | 贵州柏森香料有限公司 | Method and device for measuring reaction end point in 3, 4-methylenedioxymandelic acid synthesis reaction |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1220296A (en) * | 1997-12-14 | 1999-06-23 | 王云林 | Method for manufacturing non-dewatering urea-formaldehyde resin gum |
| CN101200529A (en) * | 2007-11-22 | 2008-06-18 | 杨素银 | Method for synthesizing environment-friendly type urea-formaldehyde plastics resin |
| CN103031095A (en) * | 2012-12-12 | 2013-04-10 | 永港伟方（北京）科技股份有限公司 | Adhesive for veneering of artificial board and preparation method of adhesive |
| CN103193947A (en) * | 2013-04-08 | 2013-07-10 | 广西大学 | Continuous protection technology of urea resin |
-
2018
- 2018-04-24 CN CN201810372030.3A patent/CN108680462A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1220296A (en) * | 1997-12-14 | 1999-06-23 | 王云林 | Method for manufacturing non-dewatering urea-formaldehyde resin gum |
| CN101200529A (en) * | 2007-11-22 | 2008-06-18 | 杨素银 | Method for synthesizing environment-friendly type urea-formaldehyde plastics resin |
| CN103031095A (en) * | 2012-12-12 | 2013-04-10 | 永港伟方（北京）科技股份有限公司 | Adhesive for veneering of artificial board and preparation method of adhesive |
| CN103193947A (en) * | 2013-04-08 | 2013-07-10 | 广西大学 | Continuous protection technology of urea resin |
Non-Patent Citations (1)
| Title |
|---|
| 郭宇鹏: "水溶性硫脲醛（WTF）重金属捕集剂的合成及应用", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111751248A (en) * | 2020-07-03 | 2020-10-09 | 贵州柏森香料有限公司 | Method and device for measuring reaction end point in 3, 4-methylenedioxymandelic acid synthesis reaction |
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Application publication date: 20181019 |