CN211329304U - Device for uniformly feeding water-soluble urea-formaldehyde resin in synthetic process - Google Patents

Device for uniformly feeding water-soluble urea-formaldehyde resin in synthetic process Download PDF

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CN211329304U
CN211329304U CN201921581744.1U CN201921581744U CN211329304U CN 211329304 U CN211329304 U CN 211329304U CN 201921581744 U CN201921581744 U CN 201921581744U CN 211329304 U CN211329304 U CN 211329304U
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feeding
pipe
reaction
reaction kettle
axis
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刘涉江
张广庆
夏云飞
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Tianjin Taimu Ecological Environment Technology Co ltd
Tianjin University
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Tianjin Taimu Ecological Environment Technology Co ltd
Tianjin University
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Abstract

The utility model relates to a device for evenly feeding materials in the process of synthesizing water-soluble urea-formaldehyde sulfide resin; 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 on two sides of the pipe and 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. The feeding pipes are distributed in the reaction kettle in a spiral mode, the spiral angle is the included angle between the tangent line outside the feeding pipes and the horizontal line, the spiral angle is 20-60 degrees, and the spiral diameter of the feeding pipes accounts for 50-70% of the diameter of the reaction kettle. The feeding pipes are uniformly distributed in the reaction kettle, so that materials on each layer can be fully mixed, and the mixing uniformity is improved by 30%.

Description

Device for uniformly feeding water-soluble urea-formaldehyde resin in synthetic process
Technical Field
The utility model belongs to water-soluble thiourea aldehyde resin synthesis field, in particular to a device that is arranged in even feeding of water-soluble urea-formaldehyde 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
Figure BDA0002210908330000011
Methylene reaction
Figure BDA0002210908330000012
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 utility model aims to overcome the defect of uneven mixing in the current water-soluble urea-formaldehyde resin synthetic process, and provide a simple process, low cost's feeding equipment and method.
The technical scheme of the utility model 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 utility model 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 utility model discloses an adopt inlet pipe evenly distributed in reation kettle, can ensure all can the intensive mixing between the material of every aspect, the not equidirectional feeding is taken in the distribution of feed inlet in addition, the inlet pipe spirals to reation kettle in the back, the direction of feed can change to realize following the purpose of all directions feeding, can follow different angles and squeeze into reation kettle with the raw materials in, realize the even mixture of material, the degree of mixing uniformity has improved 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 utility model has the main advantages that: 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 distribution diagram of the feed inlet of the present invention.
Figure 2 is the utility model discloses introduction port rotation angle schematic diagram.
FIG. 3 is a schematic view showing the rotation angle of the feed inlet.
Fig. 4 is a drawing of the uniform feeding device 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.
Adopt the utility model discloses a method of device mixing water-soluble urea-formaldehyde resin raw materials, formaldehyde is added into reation kettle, adjust pH to 7.8-8.5 after, heat to 40-60 ℃, then the thiourea aqueous solution that will heat after the mass fraction is 10-30% passes through feed liquor pump 3 and gets into inlet pipe 2, with the interior formaldehyde homogeneous mixing of reation kettle, adjust the pH value of mixed solution to 7.8-8.5 and continue to react for 20-30min, then adjust pH to 4.0-4.5, heat up to 80-90 ℃ and continue to react, and adopt turbidity titration method constantly to carry out the terminal point and judge, will synthesize the product and emit the product through drain hole 5 after the terminal point reachs. 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 finding the same water-soluble urea formaldehyde resin contrast test, use the utility model discloses device and method can make the effective content of water-soluble thiourea aldehyde resin improve, and product property can improve 37%. In addition, use the utility model discloses device and method owing to need not to reuse agitating unit, have reduced manufacturing cost, and the energy consumption of unit mass product has reduced 23%, and the while production condition changes into the liquid-liquid reaction, has increased the inter-reactant contact probability, has improved reaction rate to the even device of feeding uses and also makes reaction time shorten greatly, and reaction time has reduced 40%, has improved production efficiency.
The device and method for feeding evenly water-soluble thiourea aldehyde resin provided by the present invention have been described by way of example, and it is obvious for the relevant technical personnel to change or properly change and combine the manufacturing method described herein without departing from the content, spirit and scope of the present invention to realize the technology 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 (2)

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.
CN201921581744.1U 2019-09-23 2019-09-23 Device for uniformly feeding water-soluble urea-formaldehyde resin in synthetic process Expired - Fee Related CN211329304U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110614068A (en) * 2019-09-23 2019-12-27 天津大学 Device and method for uniform feeding in water-soluble urea-formaldehyde resin synthesis process

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110614068A (en) * 2019-09-23 2019-12-27 天津大学 Device and method for uniform feeding in water-soluble urea-formaldehyde resin synthesis process

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