CN107189059B - Polyamide solid-phase tackifying control ball and application thereof - Google Patents
Polyamide solid-phase tackifying control ball and application thereof Download PDFInfo
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- CN107189059B CN107189059B CN201710469698.5A CN201710469698A CN107189059B CN 107189059 B CN107189059 B CN 107189059B CN 201710469698 A CN201710469698 A CN 201710469698A CN 107189059 B CN107189059 B CN 107189059B
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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
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/04—Preparatory processes
- C08G69/06—Solid state polycondensation
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- 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
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
- C08G69/16—Preparatory processes
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- 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
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
- C08G69/28—Preparatory processes
- C08G69/30—Solid state polycondensation
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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
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/36—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino acids, polyamines and polycarboxylic acids
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Abstract
The invention belongs to the technical field of polymer preparation, and discloses a polyamide solid-phase tackifying control ball and application thereof. The control ball is composed of blades with one ends connected together and the other ends spherically diverging in a three-dimensional space, the blades are sequentially composed of a surface layer with a mesh structure, an inner filter screen layer and an inner space from outside to inside, inorganic particles are filled in the inner space, and the inner filter screen layer can realize gas passing and prevent leakage of the inorganic particles. The control ball blade can provide a separation layer for solid polyamide or copolyamide slices, promote the turning energy of the slices in a dynamic state, and control the polyamide or copolyamide slices in the ball to move along the blade so as to strengthen the turning of the slices; meanwhile, the adsorption can be carried out through inorganic particles in the blades, so that the overflow of water vapor in polyamide or copolyamide slices is facilitated, the effect of enhanced stirring is realized, and then the acidic gas is slowly released, so that the solid-phase tackifying process is promoted.
Description
Technical Field
The invention belongs to the technical field of polymer preparation, and particularly relates to a polyamide solid-phase tackifying control ball and application thereof.
Background
Polyamides (PA, commonly known as nylon) have been developed and industrialized by dupont in the united states for over 70 years since the 30 th century. The polyamide has good affinity and good cohesive force to a plurality of materials, and meanwhile, the polyamide has good mechanical properties, such as high strength, wear resistance, self lubrication, oil resistance, chemical resistance and the like, so the polyamide can be used as fiber, engineering plastic and has wide application prospect in industry. In order to obtain better mechanical properties, it is often necessary to increase the molecular weight of the polymer in such a way as to reduce the proportion of the polymer chain ends as much as possible, thus achieving the achievement of a high molecular weight (high viscosity) polyamide starting material.
In the polycondensation of polyamides, increasing the dwell time in the late polymerization stage directly leads to an increase in the polymer molecular weight, but leads to difficulties in the discharge of highly viscous polyamides in the molten state. Thus, there is a need to achieve the preparation of high viscosity polyamide chips by other routes. Solid phase polycondensation is a commonly used and effective method.
Solid phase polycondensation (SSP) is a polycondensation reaction carried out in a solid state, and as early as the 30 s of the 20 th century, flory found that a polycondensation reaction can continue to occur while a polyamide obtained by melt polycondensation is maintained at a certain temperature in a solid state. With the continued intensive research, it has been possible to obtain polymers of high quality, high performance and high relative molecular mass by solid phase polycondensation, especially for polycondensation processes of monomers having a very high melting point or easily decomposable above, and also for high temperature resistant polymers, solid phase polycondensation being a more important polymerization process. Solid phase polycondensation is a process in which a monomer or a prepolymer having a relatively low molecular weight is heated to a temperature higher than the glass transition temperature and a polycondensation reaction is carried out at a temperature lower than the melting point. At this time, the macromolecular chain is still in a fixed state, the terminal functional groups acquire enough activity, the macromolecular chain approaches each other through diffusion and reacts, and the generated micromolecular byproducts are brought out of the reaction system by means of vacuum or inert gas flow, so that the polycondensation reaction is promoted to be carried out positively, the molecular weight of the product is continuously improved, and finally the copolymer with high viscosity is acquired. The solid phase polycondensation is characterized as follows: (1) The reaction temperature is obviously reduced, and the by-products and degradation reactions are obviously reduced. (2) The relative molecular mass of the polymer can be obviously improved, so that the mechanical property of the polymer is improved. (3) The solid phase polycondensation temperature is lower, and stirring of high-viscosity melt is avoided, so that the energy consumption in the whole polycondensation process is reduced. (4) The solid phase polycondensation does not need solvent, and is an environment-friendly polymerization reaction. (5) the polymerization process is simple and flexible; the polymerization mode can be operated continuously or batchwise. (6) The reaction is stable, high pressure is not required, and the requirement on equipment materials is low.
In the solid-phase tackifying process, the effective removal of small molecules can lead the polycondensation reaction to proceed towards the polymerization direction, thereby being more beneficial to promoting the promotion of the solid-phase tackifying effect. Therefore, in actual industrial production, the polyamide chips to be tackified are often in a certain motion state. In addition, according to the polycondensation mechanism of polyamide, the acid environment is favorable for the polycondensation, so that the pH value atmosphere of the polycondensation environment is properly improved, and the solid-phase tackifying effect is also favorable for improvement.
The solid-phase tackifying process is generally carried out in a rotary vacuum drum (vacuum dryer) in industry, and the overturning movement of the slice is realized along with the rotation of the vacuum drum, so that the small molecules produced by polycondensation are removed, and the tackifying process is realized. But only through the rotation effect of the vacuum rotary drum, the release efficiency and the tackifying effect of the small molecules are required to be further improved.
Disclosure of Invention
In view of the above drawbacks and shortcomings of the prior art, a primary object of the present invention is to provide a polyamide solid-phase tackifying control sphere.
It is another object of the present invention to provide the use of the above solid stating control sphere in polyamide or copolyamide solid stating.
The invention aims at realizing the following technical scheme:
a polyamide solid-phase tackifying control ball is composed of blades with one end connected together and the other end spherically diverging in three-dimensional space, and is composed of surface layer with mesh structure, internal filter screen layer and internal space sequentially from outside to inside, and the internal space is filled with inorganic particles, and the internal filter screen layer can realize gas passing through while preventing leakage of inorganic particles.
Preferably, the number of blades is 3 to 12.
Preferably, the blade is in a salix-leaf structure, the length a of the blade is not smaller than the width b, the value range of a and b is 0.5-20 mm, and the torsion angle range of the blade is 10-65 degrees.
Preferably, the surface layer with the mesh structure is a stainless steel layer with the mesh structure, the mesh density is 50-800 meshes, the meshes are round, oval or rectangular, and the diameter or length and width of the meshes are 0.2-2.0 mm. The stainless steel includes, but is not limited to, 301 stainless steel, 302 stainless steel, 304 stainless steel, 309 stainless steel, 316 stainless steel, 321 stainless steel, 440 stainless steel.
Preferably, the inner filter screen layer is a high temperature resistant polymer filter screen layer, and the high temperature resistant polymer filter screen layer comprises, but is not limited to, a single layer or two or more layers with a gram weight of 40g/m 2 ～300g/m 2 Polyphenylene sulfide nonwoven fabric or woven fabric, polyacrylonitrile nonwoven fabric or woven fabric.
Preferably, the inorganic particles include, but are not limited to, citric anhydride, disodium hydrogen phosphate, sodium dihydrogen phosphate. The inorganic particles absorb moisture and then release the acidic component slowly by evaporation of the moisture.
The application of the solid-phase tackifying control ball in polyamide or copolyamide solid-phase tackifying comprises the following steps: directly mixing the control ball with polyamide or copolyamide slices to be thickened, and then entering a batch solid-phase tackifying device for solid-phase polycondensation reaction to obtain the high-viscosity polyamide or copolyamide.
The control ball has the following advantages and beneficial effects:
the control ball blade can provide a separation layer for solid polyamide or copolyamide slices, promote the turning of the slices in a dynamic state, and control the polyamide or copolyamide slices in the ball to move along the blade so as to strengthen the turning of the slices; meanwhile, the adsorption can be carried out through inorganic particles in the blades, so that the overflow of water vapor in polyamide or copolyamide slices is facilitated, the effect of enhanced stirring is realized, and then the acidic gas is slowly released, so that the solid-phase tackifying process is promoted.
Drawings
FIG. 1 is a three-view (a: front view; b left view; c: top view) of a polyamide solid-phase adhesion control sphere of example 5;
FIG. 2 is a schematic structural view (a: outline drawing; b: schematic internal structure) of a blade of a polyamide solid-phase adhesion-controlling balloon-like structure in example 5.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but embodiments of the present invention are not limited thereto.
Example 1
The polyamide solid-phase tackifying control ball of the embodiment consists of 3 blades with salix leaf-shaped structures, one ends of the blades are connected together through a central sphere, the other ends of the blades are spherically dispersed in a three-dimensional space, the length a of each blade is 20mm, the width b of each blade is 10mm, and the torsion angle of each blade is 30 degrees. The blade and the center sphere are composed of a surface layer with a mesh structure, an inner filter screen layer and an inner space. The surface layer is made of a No. 301 stainless steel layer, the mesh density is 800 meshes, and the diameter of the round mesh is 0.2mm. The inner layer of the blade uses polyphenylene sulfide non-woven fabric as a high temperature resistant non-woven fabric filter screen layer, and the gram weight of the non-woven fabric material is 300g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the The internal space uses sodium dihydrogen phosphate as inorganic particlesAfter absorbing the moisture, the slow release overflow of the acidic component is realized along with the evaporation of the moisture. The inner filter layer can realize gas passing and prevent inorganic particles from leaking.
The control ball of the embodiment is used for preparing high-viscosity copolyamide 6/66 by a batch method, and the control ball is directly mixed with copolyamide 6/66 slices to be thickened, and then enters a batch solid-phase tackifying device for solid-phase polycondensation reaction to obtain high-viscosity polyamide or copolyamide. The results showed that the relative viscosity of copolyamide 6/66 increased from 2.8 to 4.0 in a vacuum rotary dryer drum at 165℃for 16 to 24 hours. The time for realizing the same tackifying effect under the same drying equipment and drying temperature without adding the control ball is 32-40 hours.
Example 2
The polyamide solid-phase tackifying control ball of the embodiment consists of 12 blades with salix leaf-shaped structures, one ends of the blades are connected together through a central sphere, the other ends of the blades are spherically dispersed in a three-dimensional space, the length a of each blade is 0.5mm, the width b of each blade is 0.5mm, and the torsion angle of each blade is 10 degrees. The blade and the center sphere are composed of a surface layer with a mesh structure, an inner filter screen layer and an inner space. The surface layer is made of 304 # stainless steel, the mesh density is 50 meshes, the major axis diameter of the elliptical mesh is 1.0mm, and the minor axis diameter is 0.4mm. The inner layer of the blade uses two layers of polyacrylonitrile non-woven fabrics as a high temperature resistant non-woven fabric layer filter screen, and the gram weight of the non-woven fabric material is 40g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the The internal space uses disodium hydrogen phosphate and sodium dihydrogen phosphate (the mass ratio is 1:1) as inorganic particles, and the slow release overflow of the acidic components is realized along with the evaporation of the moisture after the moisture is absorbed. The inner filter layer can realize gas passing and prevent inorganic particles from leaking.
The control ball of this example is used for preparing high-viscosity polyamide 66 by batch process, the control ball is directly mixed with polyamide 66 slice to be thickened, and then enters into batch solid-phase tackifying device to carry out solid-phase polycondensation reaction, thus obtaining high-viscosity polyamide or copolyamide. The results showed that the relative viscosity of polyamide 66 increased from 2.8 to 4.0 in a vacuum rotary dryer drum at 245℃for 18 to 24 hours. The time for realizing the same tackifying effect under the same drying equipment and drying temperature without adding the control ball is 32-40 hours.
Example 3
The polyamide solid-phase tackifying control ball of the embodiment is composed of 12 blades with salix leaf-shaped structures, one ends of the blades are connected together through a central sphere, the other ends of the blades are spherically dispersed in a three-dimensional space, the length a of each blade is 20mm, the width b of each blade is 15mm, and the torsion angle of each blade is 45 degrees. The blade and the center sphere are composed of a surface layer with a mesh structure, an inner filter screen layer and an inner space. The surface layer is a No. 302 stainless steel layer, the mesh density is 600 meshes, and the length and the width of the rectangular mesh are divided into 2.0mm and 0.5mm. The inner layer of the blade uses polyphenylene sulfide warp-weft knitted fabric as a high-temperature resistant filter screen layer, and the gram weight of the knitted fabric material is 250g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the The internal space uses sodium dihydrogen phosphate as inorganic particles, and the slow release overflow of acidic components is realized along with the evaporation of moisture after moisture is absorbed. The inner filter layer can realize gas passing and prevent inorganic particles from leaking.
The control ball of the embodiment is used for preparing high-viscosity copolyamide 6/66/10 by a batch method, and the control ball is directly mixed with copolyamide 6/66/10 slices to be thickened and then enters a batch solid-phase tackifying device for solid-phase polycondensation reaction to obtain the high-viscosity polyamide or copolyamide. The results showed that the relative viscosity of copolyamide 6/66/10 increased from 2.8 to 4.0 in a vacuum rotary dryer drum at 230℃for 16 to 24 hours. The time for realizing the same tackifying effect under the same drying equipment and drying temperature without adding the control ball is 32-40 hours.
Example 4
The polyamide solid-phase tackifying control ball of the embodiment consists of 8 blades with salix leaf-shaped structures, one ends of the blades are connected together through a central sphere, the other ends of the blades are spherically dispersed in a three-dimensional space, the length a of each blade is 16mm, the width b of each blade is 10.8mm, and the torsion angle of each blade is 60 degrees. The blade and the center sphere are composed of a surface layer with a mesh structure, an inner filter screen layer and an inner space. The surface layer is made of 309 # stainless steel, the mesh density is 400 meshes, and the diameter of the round mesh is 0.8mm. The inner layer of the blade uses two layers of polyphenylene sulfide non-woven fabrics as high temperature resistant non-woven fabricsCloth layer filter screen, gram weight of single layer non-woven fabric material is 100g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the The inner space uses citric anhydride as inorganic particles, and the slow release overflow of the acidic component is realized along with the evaporation of the moisture after the moisture is absorbed. The inner filter layer can realize gas passing and prevent inorganic particles from leaking.
The control ball of the embodiment is used for preparing high-viscosity copolyamide 6/12 by a batch method, and the control ball is directly mixed with copolyamide 6/12 slices to be thickened and then enters a batch solid-phase tackifying device for solid-phase polycondensation reaction to obtain high-viscosity polyamide or copolyamide. The results showed that the relative viscosity of copolyamide 6/12 increased from 2.8 to 4.0 in a vacuum rotary dryer drum at 140℃for 20 to 28 hours. The time for realizing the same tackifying effect under the same drying equipment and drying temperature without adding the control ball is 32-40 hours.
Example 5
The three views of the polyamide solid-phase tackifying control ball are shown in fig. 1 (a: front view; b: left view; c: top view), and the polyamide solid-phase tackifying control ball is composed of 10 blades with salix-leaf structures, one ends of the blades are connected together through a central sphere, and the other ends of the blades are spherically dispersed in a three-dimensional space. The structural schematic diagram of the blade with the salix-shaped structure is shown in fig. 2 (a: outline drawing; b: internal structure schematic diagram), the length a of the blade is 20mm, the width b of the blade is 8mm, and the torsion angle 2 theta of the blade is 65 degrees. The blade and the center sphere are composed of a surface layer with a mesh structure, an inner filter screen layer and an inner space. The surface layer is made of 440 # stainless steel, the mesh density is 600 meshes, and the diameter of the round mesh is 0.4mm. The inner layer of the blade uses polyacrylonitrile warp and weft knitted fabric as a high-temperature resistant filter screen layer, and the gram weight of the knitted fabric material is 240g/m 2 The method comprises the steps of carrying out a first treatment on the surface of the The internal space uses sodium dihydrogen phosphate as inorganic particles, and the slow release overflow of acidic components is realized along with the evaporation of moisture after moisture is absorbed. The inner filter layer can realize gas passing and prevent inorganic particles from leaking.
The control ball of the embodiment is used for preparing the high-viscosity polyamide 6 by a batch method, and the control ball is directly mixed with the polyamide 6 slice to be thickened, and then enters a batch solid-phase tackifying device for solid-phase polycondensation reaction to obtain the high-viscosity polyamide or copolyamide. The results showed that the relative viscosity of polyamide 6 increased from 2.8 to 4.0 in a vacuum rotary dryer drum at 210℃for 16 to 24 hours. The time for realizing the same tackifying effect under the same drying equipment and drying temperature without adding the control ball is 32-40 hours.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (4)
1. A polyamide solid-phase tackifying control ball is characterized in that: the control ball is composed of blades with one end connected together and the other end spherically divergent in a three-dimensional space, the blades are sequentially composed of a surface layer with a mesh structure, an inner filter screen layer and an inner space from outside to inside, inorganic particles are filled in the inner space, and the inner filter screen layer can realize gas passing and prevent leakage of the inorganic particles;
the blade is of a salix leaf-shaped structure, the length a of the blade is not smaller than the width b, the value range of a and b is 0.5-20 mm, and the torsion angle range of the blade is 10-65 degrees;
the inorganic particles are citric anhydride, disodium hydrogen phosphate or sodium dihydrogen phosphate;
the number of the blades is 3-12.
2. The polyamide solid-phase tackifying control sphere according to claim 1, characterized in that: the surface layer with the mesh structure is a stainless steel layer with the mesh structure, the mesh density is 50-800 meshes, the meshes are round, oval or rectangular, and the diameter or length and width of the meshes are 0.2-2.0 mm.
3. The polyamide solid-phase tackifying control sphere according to claim 1, characterized in that: the inner filter screen layer is a single layer or two layers, and the gram weight of the inner filter screen layer is 40g +.m 2 ～300g/m 2 Polyphenylene sulfide nonwoven fabric or woven fabric, polyacrylonitrile nonwoven fabric or woven fabric.
4. Use of a polyamide solid-phase adhesion control sphere according to any one of claims 1 to 3 in polyamide or copolyamide solid-phase adhesion, characterized in that the application process is: directly mixing the control ball with polyamide or copolyamide slices to be thickened, and then entering a batch solid-phase tackifying device for solid-phase polycondensation reaction to obtain the high-viscosity polyamide or copolyamide.
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2017
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| US3816369A (en) * | 1971-11-08 | 1974-06-11 | Ici Ltd | Process for the preparation of polyamides with alkali metal dihydrogen orthophosphate as catalyst |
| JP2010215682A (en) * | 2009-03-13 | 2010-09-30 | Mitsubishi Gas Chemical Co Inc | Method for solid state polymerization of polyamide |
| JP2011057929A (en) * | 2009-09-14 | 2011-03-24 | Mitsubishi Gas Chemical Co Inc | Polyamide resin composition |
| CN102391489A (en) * | 2011-09-01 | 2012-03-28 | 大连海新工程技术有限公司 | Reactor integrating stirring, preheating and solid-phase viscosity increasing of polyester |
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