CN110614068A - Device and method for uniform feeding in water-soluble urea-formaldehyde resin synthesis process - Google Patents
Device and method for uniform feeding in water-soluble urea-formaldehyde resin synthesis process Download PDFInfo
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- CN110614068A CN110614068A CN201910898245.3A CN201910898245A CN110614068A CN 110614068 A CN110614068 A CN 110614068A CN 201910898245 A CN201910898245 A CN 201910898245A CN 110614068 A CN110614068 A CN 110614068A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08G12/02—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
- C08G12/04—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with acyclic or carbocyclic compounds
- C08G12/10—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with acyclic or carbocyclic compounds with acyclic compounds having the moiety X=C(—N<)2 in which X is O, S or —N
- C08G12/12—Ureas; Thioureas
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Abstract
The invention relates to a device and a method for uniformly feeding in a water-soluble urea-formaldehyde sulfide resin synthesis process. The device comprises a reaction kettle, a feeding pipe, a feeding pump, a feeding port and a discharging port; the tail end of the feeding pipe is closed; the feeding ports are distributed on the feeding pipe; the position of the feed inlet is described under the condition that the feed inlet pipe is vertically arranged, a through hole is arranged at any position of two sides of the feed inlet pipe, which is vertical to the axis of the pipe, and another through hole is arranged at the interval of 5-15 cm along the axis of the feed inlet pipe, and the through hole rotates 30-60 degrees along the angle of the axis, and the aperture is 0.5-1 cm. The feeding pipes are distributed in a spiral mode in the reaction kettle. The formaldehyde is added into the reaction kettle, the solution can be mixed more uniformly due to the distribution of the feeding holes and the advantage of large quantity, the side reaction in the resin synthesis process is reduced, and the performance of the product is improved by 37%. Meanwhile, the device has uniform feeding, reduces the reaction time by 40 percent and improves the production efficiency.
Description
Technical Field
The invention belongs to the field of synthesis of water-soluble thiourea aldehyde resin, and particularly relates to a device and a method for uniformly feeding in a water-soluble thiourea aldehyde resin synthesis process.
Background
The water-soluble urea-formaldehyde resin is a water-soluble high-molecular heavy metal chelating agent containing sulfur groups, and the main functional group for stabilizing heavy metal pollutants in soil is a sulfur bond, so that the passivation effect is obvious. The synthesis process is an amine-formaldehyde reaction, also called Cannizzaro reaction, which mainly comprises two stages of reactions, wherein the first stage is an addition reaction called hydroxymethylation; the second stage is polycondensation reaction, the reaction speed of the hydroxymethylation reaction is higher under neutral and alkalescent conditions, and the reaction speed of the polycondensation reaction is higher under acidic conditions. During the polycondensation reaction, most of the hydroxymethyl groups are dehydrated to form methylene groups, and a small number of the hydroxymethyl groups form methylene ether bonds, so the polycondensation reaction also becomes a methylenation reaction. The reaction equation is as follows:
hydroxymethylation reaction
Methylene reaction
The specific experimental steps and reaction conditions are shown in Guoguppeng patent "a preparation method of a water-soluble thiourea aldehyde heavy metal trapping agent with low formaldehyde content" (CN201510808974.7), formaldehyde is usually added into a reaction kettle, and then thiourea is added into the reaction kettle for reaction. The specific method comprises the following steps: adding formaldehyde into a reactor, heating to 60-80 ℃, directly pouring thiourea and formaldehyde into the reactor according to the proportion for mixing, adjusting the pH value to 7.5-9.5 by using NaOH solution, reacting for 20-50min at 60-80 ℃, adjusting the pH value to 4.0-6.0 by using HCl solution, heating to 75-95 ℃, continuously reacting for more than 50min, keeping the pH value between 4.0-6.0, and stopping heating when the reaction reaches the end point by adopting a turbidity titration method.
Since the reaction is rapid during the synthesis and side reactions proceed, strict requirements are imposed on the concentration distribution between the starting materials. In the traditional method, magnetic stirring is adopted for stirring, the upper part of a reactor is not fully stirred, so that the reaction conditions in the reactor are not uniform, reaction substances are directly added from the top of the reactor, solid reactants in the reactor are dissolved in a large amount just after being added into the reactor, the concentration at the upper part of the reactor is too high, the reaction process is influenced, side reactions are generated, the concentration at the bottom of the reaction kettle is relatively low, the reaction is not fully performed, and the side reactions are also generated, so that the whole reaction process and the product performance in the reactor are influenced.
Disclosure of Invention
The invention aims to overcome the defect of uneven mixing in the current water-soluble urea-formaldehyde sulfide resin synthesis process, and provides a feeding device and a feeding method which are simple in process and low in cost.
The technical scheme of the invention is as follows:
a device for uniformly feeding in the synthesis process of water-soluble urea-formaldehyde resin comprises a reaction kettle 1, a feeding pipe 2, a feeding pump 3, a feeding hole 4 and a discharging hole 5; the end of the feeding pipe 2 is closed; the feeding ports 4 are distributed on the feeding pipe 2; the position of the feed inlet 4 is described under the condition that the feed pipe is vertically placed, the feed inlet 4 is provided with a through hole at any position on two sides of the pipe, which is vertical to the axis of the pipe, the other through holes are provided with through holes at intervals of 5-15 cm along the axis of the feed pipe, the through holes rotate 30-60 degrees along the axis, and the aperture is 0.5-1 cm.
The feeding pipes are distributed in the reaction kettle in a spiral mode, the helix angle is an included angle between the external tangent line of the feeding pipes and the horizontal line, the helix angle is an angle of 20-60 degrees, and the spiral diameter of the feeding pipes accounts for 50-70% of the diameter of the reaction kettle.
The device of the invention is used for synthesizing the water-soluble thiourea aldehyde resin; adding formaldehyde into a reaction kettle, adjusting the pH value to 7.8-8.5, heating to 40-60 ℃, then feeding the heated thiourea aqueous solution with the mass fraction of 10-30% into a feeding pipe 2 through a liquid inlet pump 3, uniformly mixing with the formaldehyde in the reaction kettle, adjusting the pH value of the mixed solution to 7.8-8.5, continuing to react for 20-30min, then adjusting the pH value to 4.0-4.5, heating to 80-90 ℃, continuing to react until the end point, and discharging the synthesized product through a discharge port 5 to obtain the product.
The feeding pipes are uniformly distributed in the reaction kettle, so that the materials on each layer can be fully mixed, in addition, the distribution of the feeding holes adopts feeding in different directions, after the feeding pipes are coiled into the reaction kettle, the feeding direction can be changed, so that the purpose of feeding in all directions is realized, the raw materials can be thrown into the reaction kettle from different angles, the uniform mixing of the materials is realized, and the mixing uniformity is improved by 30%. The improvement of the uniformity of the mixed materials requires more precise condition control in the reaction kettle and more precise pH and temperature regulation so as to reduce the occurrence of side reactions. Therefore, the device can efficiently improve the uniformity of materials, improve the uniformity of reactants, be beneficial to reducing the generation of side reactions and reduce the reaction time.
The main advantages of the invention are: in the reation kettle was added to formaldehyde, in adding inlet pipe 2 with thiourea through the charge-in pump after adjusting pH, then mix through feed inlet 4 and formaldehyde, the distribution of feed inlet and the great advantage of quantity make can mix more evenly between the solution, the going on of the side reaction in the resin synthesis process has been reduced, and formulate the solid in the raw materials into reaction solution, be favorable to fully contacting between the reactant, can not produce the too high problem of local concentration, the performance that has improved the product reaches 37%. Meanwhile, the contact area between reactants is large during liquid-liquid reaction, and the feeding of the device is uniform, so that the reaction time is reduced by 40 percent, and the production efficiency is improved.
Drawings
FIG. 1 is a feed gap profile of the present invention.
FIG. 2 is a schematic view of the rotation angle of the injection port of the present invention.
FIG. 3 is a schematic view showing the rotation angle of the feed inlet.
FIG. 4 is a view of a uniform feeding apparatus of the present invention.
Reference numerals: 1. a reaction kettle; 2. a feed pipe; 3. a feed pump; 4. a feed inlet; 5. a discharging port; l1 and L2 are auxiliary lines and are connecting lines formed by the centers of the circle of the feed inlet, and an included angle alpha formed by the two line segments is the rotation angle of the feed inlet; the included angle beta between the outer tangent of the feeding pipe and the horizontal line is the helix angle of the feeding pipe.
Detailed Description
The invention will be further described with reference to the accompanying drawings:
as shown in figures 1-4, the device comprises a reaction kettle 1, a feeding pipe 2, a feeding pump 3, a feeding port 4 and a discharging port 5, wherein the tail end of the feeding pipe 2 is closed, so that reaction liquid can only enter the reaction kettle from the feeding port 4, and the reaction liquid is uniformly mixed. After the pH value of formaldehyde is regulated, the formaldehyde is pumped into a reaction kettle 1 through a liquid inlet pump, then a thiourea solution liquid inlet pump 3 enters a feeding pipe 2, and feeding holes 4 with different diameters are distributed on the surface of the feeding pipe, and the feeding holes are distributed as follows: under the condition that a feeding pipe is vertically placed, a through hole is drilled at a position, perpendicular to the axis of the pipe, of one of two sides of the pipe, then the through hole is drilled downwards along the feeding pipe at an interval of 5-15 cm, the angle of the axis of the through hole is rotated by 30-60 degrees, the aperture is 0.5-1 cm, so that the uniform feeding is ensured, the feeding pipes are distributed in a spiral downward mode in a reaction kettle, the spiral rising angle is the included angle between the external tangent line of the feeding pipe and the horizontal line, the spiral rising angle is 20-60 degrees, and the spiral diameter of the feeding pipe accounts for 50-70% of the diameter of the reaction kettle, so that the feeding pipe has a large feeding area in the reaction kettle, the uniform mixing of formaldehyde and thiourea solution on different layers of the reaction kettle is ensured, and the tail end of the feeding pipe is closed. The mode of adopting the feed inlet feeding can effectual improvement uniformity between the material, is favorable to proportional reaction between the reactant, avoids the formation of reaction accessory substance.
The method for mixing the water-soluble urea-formaldehyde-sulfur resin raw material by adopting the device comprises the steps of adding formaldehyde into a reaction kettle, adjusting the pH value to 7.8-8.5, heating to 40-60 ℃, then feeding thiourea aqueous solution with the mass fraction of 10-30% after heating into a feeding pipe 2 through a liquid inlet pump 3, uniformly mixing with the formaldehyde in the reaction kettle, adjusting the pH value of the mixed solution to 7.8-8.5, continuing to react for 20-30min, adjusting the pH value to 4.0-4.5, heating to 80-90 ℃, continuing to react, continuously performing end point judgment by adopting a turbidity titration method, and discharging the synthesized product through a discharge port 5 after the end point is reached. Because new reaction conditions are adopted, the reaction time is greatly shortened, the solid in the raw materials is prepared into reaction solution, the full contact between reactants is facilitated, the problem of overhigh local concentration is avoided, the side reaction rate is obviously reduced, and the product performance is improved.
The specific examples are illustrated below:
example 1: a device and a method for uniformly feeding in a water-soluble urea-formaldehyde resin synthesis process are characterized in that feeding pipes are distributed in a way that a through hole is formed in one position on two sides of a pipe, which is perpendicular to the axis of the pipe, under the condition that the feeding pipes are vertically placed, the through hole is formed in the position, which is 15 cm away from the two sides of the pipe, the through hole is formed downwards along the feeding pipes, the angle of the axis of the through hole is rotated by 30 degrees, the aperture size is 0.5 cm, the helix angle of the feeding pipes is 60 degrees, and the helix diameter is 50% of the diameter of a reaction kettle, formaldehyde is added into the reaction kettle after the pH value of the formaldehyde is adjusted, thiourea solution is added into the reaction kettle, the reaction. The heavy metal adsorption capacity of the final product is improved by 27 percent, which is superior to the conventional synthesis device and method of the water-soluble thiourea aldehyde resin.
Example 2: a device and a method for uniformly feeding in a water-soluble urea-formaldehyde resin synthesis process are characterized in that feeding pipes are distributed in a way that a through hole is formed in one position on two sides of a pipe, which is perpendicular to the axis of the pipe, under the condition that the feeding pipes are vertically placed, the through hole is formed in a way that the position of one position on two sides of the pipe is perpendicular to the axis of the pipe, then the through hole is formed downwards along the feeding pipes at a distance of 7.5 cm, the angle of the axis of the through hole rotates by 45 degrees, the aperture size is 0.8 cm, the helix angle of the feeding pipes is 30 degrees, the helix diameter is 60 percent of the diameter of a reaction kettle, formaldehyde is added into the reaction kettle after the pH value of the formaldehyde is adjusted. The heavy metal adsorption capacity of the final product is improved by 37 percent, which is superior to the conventional synthesis device and method of the water-soluble thiourea aldehyde resin.
Example 3: a device and a method for uniformly feeding in a water-soluble urea-formaldehyde resin synthesis process are characterized in that feeding pipes are distributed in a way that a through hole is formed in one position on two sides of a pipe, which is perpendicular to the axis of the pipe, under the condition that the feeding pipes are vertically placed, the through hole is formed in a position which is 10 cm away from the feeding pipes downwards, the angle of the axis of the through hole is rotated by 60 degrees, the aperture is 0.75 cm, the helix angle of the feeding pipe is 50 degrees, and the helix diameter is 70 percent of the diameter of a reaction kettle, formaldehyde is added into the reaction kettle after the pH value of the formaldehyde is adjusted, thiourea solution is added into the reaction kettle, the reaction kettle is heated to 50 ℃, the reaction is continued until the end point is. The heavy metal adsorption capacity of the final product is improved by 34 percent, which is superior to the conventional synthesis device and method of the water-soluble thiourea aldehyde resin.
Example 4: a device and a method for uniformly feeding in a water-soluble urea-formaldehyde resin synthesis process are characterized in that feeding pipes are distributed, a through hole is drilled on the axis of a vertical pipe at one position on two sides of the pipe under the condition that the feeding pipes are vertically placed, then the through hole is drilled at the interval of 5 cm downwards along the feeding pipes, the angle of the axis of the through hole is rotated by 50 degrees, the aperture is 0.9 cm, the helix angle of the feeding pipes is 60 degrees, the helix diameter is 60 percent of the diameter of a reaction kettle, formaldehyde is added into the reaction kettle after the pH value of the formaldehyde is adjusted, thiourea solution is added into the reaction kettle, the reaction kettle is heated to 50 ℃, the reaction is continued until the end point is determined, the reaction is stopped. The heavy metal adsorption capacity of the final product is improved by 30 percent, which is superior to the conventional synthesis device and method of the water-soluble thiourea aldehyde resin.
In the synthesis process, the formaldehyde solution is added into a reaction kettle 1 after being subjected to pH adjustment, the mixture is heated to 40-60 ℃, the heated thiourea aqueous solution with the mass fraction of 10-30% is adjusted to the pH value of 7.8-8.5 and then enters a feed pipe 2 through a liquid inlet pump 3 to be uniformly mixed with formaldehyde in the reaction kettle, the pH value of the mixed solution is adjusted to 7.8-8.5, the reaction is continued for 20-30min, the pH value is adjusted to 4.0-4.5, the temperature is increased to 80-90 ℃, the reaction is continued, the end point judgment is continuously carried out, and the synthesized product is discharged through a discharge port 5 after the end point is reached.
Through a comparison test on the same water-soluble thiourea-formaldehyde resin, the device and the method disclosed by the invention can improve the effective content of the water-soluble thiourea-formaldehyde resin and improve the product performance by 37%. In addition, by using the device and the method, a stirring device is not needed, so that the production cost is reduced, the energy consumption of a unit mass product is reduced by 23%, meanwhile, the production condition is changed into liquid-liquid reaction, the contact probability among reactants is increased, the reaction rate is improved, the reaction time is greatly shortened due to the use of the device with uniform feeding, the reaction time is reduced by 40%, and the production efficiency is improved.
The apparatus and method for uniformly feeding a water-soluble thiourea aldehyde resin, which are proposed by the present invention, have been described by way of example, and it is obvious to those skilled in the art that the technique of the present invention can be implemented by modifying or appropriately changing and combining the manufacturing method described herein without departing from the content, spirit and scope of the present invention. It is expressly intended that all such similar substitutes and modifications apparent to those skilled in the art are deemed to be within the spirit, scope and content of the invention.
Claims (3)
1. A device for uniformly feeding in the synthesis process of water-soluble urea-formaldehyde resin comprises a reaction kettle (1), a feeding pipe (2), a feeding pump (3), a feeding port (4) and a discharging port (5), and is characterized in that the tail end of the feeding pipe (2) is closed; the feed inlets (4) are distributed on the feed pipe (2); the position of the feed inlet (4) is described under the condition that the feed pipe is vertically placed, a through hole is arranged at any position of two sides of the feed pipe, which is vertical to the axis of the pipe, other through holes are arranged at intervals of 5-15 cm along the axis of the feed pipe, the through hole rotates 30-60 degrees along the axis, and the aperture is 0.5-1 cm.
2. The apparatus as claimed in claim 1, wherein the feed pipes are distributed in a spiral manner in the reaction vessel, the helix angle is an angle between a tangent of the feed pipe and a horizontal line, the helix angle is 20 to 60 degrees, and the spiral diameter of the feed pipe accounts for 50 to 70 percent of the diameter of the reaction vessel.
3. A method for synthesizing a water-soluble thiourea aldehyde resin using the apparatus of claim 1; the method is characterized in that formaldehyde is added into a reaction kettle, the pH value is adjusted to 7.8-8.5, then the mixture is heated to 40-60 ℃, thiourea aqueous solution with the mass fraction of 10-30% enters a feeding pipe through a liquid inlet pump after being heated, the thiourea aqueous solution is uniformly mixed with the formaldehyde in the reaction kettle, the pH value of the mixed solution is adjusted to 7.8-8.5, the mixture is continuously reacted for 20-30min, then the pH value is adjusted to 4.0-4.5, the temperature is increased to 80-90 ℃, the reaction is continuously carried out until the end point is reached, and a synthetic product is discharged through a discharging port to obtain the product.
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| CN201910898245.3A CN110614068A (en) | 2019-09-23 | 2019-09-23 | Device and method for uniform feeding in water-soluble urea-formaldehyde resin synthesis process |
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| CN201910898245.3A CN110614068A (en) | 2019-09-23 | 2019-09-23 | Device and method for uniform feeding in water-soluble urea-formaldehyde resin synthesis process |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115215736A (en) * | 2022-08-11 | 2022-10-21 | 山东海科创新研究院有限公司 | Low-phenolic-ratio bisphenol F synthesis process |
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