CA2324885A1 - Polyesters - Google Patents
Polyesters Download PDFInfo
- Publication number
- CA2324885A1 CA2324885A1 CA002324885A CA2324885A CA2324885A1 CA 2324885 A1 CA2324885 A1 CA 2324885A1 CA 002324885 A CA002324885 A CA 002324885A CA 2324885 A CA2324885 A CA 2324885A CA 2324885 A1 CA2324885 A1 CA 2324885A1
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- CA
- Canada
- Prior art keywords
- aerosol
- doped
- silica
- preparation
- silicon dioxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Abandoned
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Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/62—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
-
- 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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Health & Medical Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Silicon Compounds (AREA)
- Polyesters Or Polycarbonates (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Artificial Filaments (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
Polyesters are prepared by the known route, in which a glycol is esterified with an organic acid and the glycol contains a pyrogenically prepared silicon dioxide doped by means of aerosol.
The polyester can be used for the production of fibres.
The polyester can be used for the production of fibres.
Description
990006 FA/al Polyesters The invention relates to polyesters, a process for their preparation and their use.
Polyesters are known compounds which can be used inter alia for the production of textiles.
They are described in Ullmann's Encyclopedia of Industrial Chemistry vol A 21 (1992) pages 227 to 251.
The preparation of polyester fibres is known from Ullmann's Encyclopedia of Industrial Chemistry vol A 10 (1992) pages 579 to 613.
A glycol, inter alia, is employed as the alcohol in the preparation of polyesters or polyester fibres.
A filler is added to this glycol in order to establish certain physico-chemical properties of the polymer.
The invention provides polyesters, which are characterized in that they contain a silicon dioxide doped by means of aerosol.
A silicon dioxide doped with aluminium oxide by means of aerosol, such as is described in the patent application DE
19847161.0-41, can be employed as pyrogenically prepared silicon dioxide doped by means of aerosol.
The pyrogenically prepared silicon dioxide doped with aluminium oxide by means of aerosol is characterized in that the base component is a silica which is prepared pyrogenically in the manner of flame oxidation or, preferably, flame hydrolysis and is doped with a doping component of 1~10-4 and up to 20 wt.%, the amount of doping preferably being in the range from 1 to 10,000 ppm and the doping component being a salt or a salt mixture of aluminium or a suspension of an aluminium compound or 990006 FA/al metallic aluminium or mixtures thereof, the BET surface area of the doped oxide being between 5 and 600 m2/g, preferably in the range between 40 and 100 m2/g.
The doped silica can have a DBP number of less than 100g/100g.
The pyrogenically prepared silicon dioxide doped with aluminium oxide by means of aerosol can be prepared by feeding an aerosol into a flame such as is used for the pyrogenic preparation of silica in the manner of flame oxidation or, preferably, flame hydrolysis, mixing the -aerosol homogeneously with the gas mixture of the flame oxidation or flame hydrolysis before the reaction, subsequently allowing the aerosol-gas mixture to react in the flame and separating the resulting pyrogenically prepared silicas doped with aluminium oxide by means of aerosol off from the gas stream in a known manner, an aqueous solution which comprises salts or salt mixtures of aluminium or the metal itself in dissolved or suspended form or mixtures thereof being used for the preparation of the aerosol, and the aerosol being prepared by atomization by means of a two-component nozzle or by another method of aerosol preparation, preferably by an aerosol generator after ultrasonic atomization.
Salts which can be employed are: A1C13, Alz (SO9) 3, A1 (N03) 3-The processes of flame hydrolysis for the preparation of pyrogenic oxides and thus also for the preparation of silicon dioxide (silica) are known from Ullmanns Enzyklopadie der technischen Chemie [Ullmann's Encyclopaedia of Industrial Chemistry), 4th edition, volume 21, page 464.
According to the invention, mixtures of 0.1 to 100 per cent of the silicas which can be employed according to the invention with other pyrogenically prepared or precipitated 990006 FA/al silicas or bentonites or other conventional fillers in the preparation of polyesters or mixtures of these fillers can be employed.
The silica according to the invention which can be employed, which is obtained as the product, for example, using aluminium chloride salts dissolved in water for the preparation of the aerosol to be fed in, can be dispersed extremely well in polar media, such as e. g. water.
The polyester according to the invention is suitable for the production of fibres (polyester fibres). .
The invention also provides a process for the preparation of polyesters, in which glycol, preferably ethylene glycol, is esterified with an organic acid by a known route, which is characterized in that a pyrogenically prepared silicon dioxide doped by means of aerosol is added to the glycol.
The invention also provides a glycol, preferably ethylene glycol, which is characterized in that it contains a pyrogenically prepared silicon dioxide doped by means of aerosol, optionally up to max. 60 parts per part of glycol.
In a preferred embodiment of the invention, the glycol can contain the pyrogenically prepared silicon dioxide doped by means of aerosol in a concentration of 50 to 60 parts per part of glycol.
The preparation of the polyester can be carried out by a known route, such as is described in Ullmann's Encyclopedia of Industrial Chemistry, vol. A21 (1992) pages 227 to 251.
The production of the polyester fibres can be carried out by a known route, such as is described in Ullmann's Encyclopedia of Industrial Chemistry vol. A10 (1992) pages 579 to 613.
990006 FA/al According to the invention, the silicon dioxide doped with aluminium oxide by means of aerosol in the polyester fibres, which can have a diameter of 10 ~m diameter, can have an average particle size of 0.5 Vim.
The silicon dioxide according to the invention which can be employed and the process for its preparation and its use are explained and described in more detail with the aid of figure 1 and the following examples:
Figure 1 shows a diagram of the doping apparatus. The core piece of the apparatus is a burner of known construction for the preparation of pyrogenic oxides.
The burner 1 comprises the central pipe 2 which ends in the nozzle 3, from which the main gas stream flows out into the burner chamber and burns off there. The nozzle 3 is surrounded by the annular nozzle 4, out of which (ring or secondary) hydrogen flows.
In the central pipe 2 is the axial pipe 5, which ends a few centimetres before the nozzle of the central pipe 2. The aerosol is fed into the axial pipe 5.
The aerosol, which comprises an aqueous aluminium chloride solution, is produced in the aerosol generator 6 (ultrasonic atomizer).
The aluminium chloride-water aerosol produced in the aerosol generator 6 is passed by means of a light carrier gas stream through the heating zone 7, in which the water carried along evaporates, small salt crystals in finely divided form remaining in the gas phase.
Example 1 Preparation of a pyrogenically prepared silica of low BET
surface area doped with aluminium oxide by means of aerosol 990006 FA/al 5.25 kg/h SiCl9 are vaporized at approx. 130 °C and transferred into the central pipe 2 of the burner 1.
3.47 Nm3/h (primary) hydrogen and 3.76 Nm3/h air are additionally fed into the central pipe 2. 0.95 Nm3/h oxygen 5 are additionally added to this mixture.
The gas mixture flows out of the nozzle 3 of the burner 1 and burns in the burner chamber and the water-cooled flame pipe connected thereto.
0.5 Nm3/h (jacket or secondary) hydrogen and 0.3 Nm3/h nitrogen are fed into the annular nozzle 4.
Nm3/h (secondary) air are also additionally fed into the burner chamber.
The second gas stream flows out of the axial pipe 5 into the central pipe 2.
15 The second gas stream comprises the aerosol, which is produced in the aerosol generator 6 by ultrasonic atomization of A1C13 solution. The aerosol generator 6 atomizes here 460 g/h 2.29 per cent aqueous aluminium trichloride solution. The aluminium chloride aerosol is led 20 with the aid of the carrier gas of 0.5 Nm3/h air through the heated line, the aqueous aerosol being converted into a gas and a salt crystal aerosol at temperatures of approx.
180 °C.
At the burner mouth the temperature of the gas mixture (SiClq-air-hydrogen, water-aerosol) is 156 °C.
The reaction gases and the pyrogenic silica doped with aluminium oxide by means of aerosol are sucked through the cooling system by applying a reduced pressure. As a result of this, the particles-gas stream is cooled to approx. 100 to 160 °C. The solid is separated off from the waste gas stream in a cyclone.
990006 FA/al The pyrogenically prepared sil,'_ca doped with aluminium oxide by means of aerosol is obtained as a white finely divided powder.
In a further step, still adhering hydrochloric acid residues are removed from the silica by treatment with air containing steam at elevated temperature.
The BET surface area of the pyrogenic silica doped with aluminium oxide is 55 m2/g.
The preparation conditions are summarized in table 1.
Further analytical data of the silica according to the invention are given in table 2.
Example 2 Preparation of a pyrogenically prepared silica of high BET
surface area doped with aluminium oxide by means of aerosol 4.44 kg/h SiCl4 are vaporized at approx. 130 °C and transferred into the central pipe 2 of the burner 1 of known construction. 3.15 Nm3/h (primary) hydrogen and 8.2 Nm3/h air are additionally fed into the central pipe 2.
The gas mixture flows out of the nozzle 3 of the burner 1 and burns in the burner chamber and the water-cooled flame pipe connected thereto.
0.5 Nm3/h (jacket or secondary) hydrogen and 0.3 Nm3/h nitrogen are fed into the annular nozzle 4.
12 Nm3/h (secondary) air are also additionally fed into the burner chamber.
The second gas stream flows out of the axial pipe 5 into the central pipe 2.
The second gas stream comprises_the aerosol, which is produced in the separate atomizing unit 6 by ultrasonic 990006 FA/al atomization of A1C13 solution. The aerosol generator 6 atomizes here 450 g/h 2.29 per cent aqueous aluminium trichloride solution. The aluminium chloride aerosol is led with the aid of the carrier gas~of 0.5 Nm3/h air through the heated line, the aqueous aerosol being converted into a gas and a salt crystal aerosol at temperatures of approx.
180 °C.
At the burner mouth the temperature of the gas mixture (SiCl9-air-hydrogen, water-aerosol) is 180 °C.
The reaction gases and the pyrogenically prepared silica doped with aluminium oxide by means of aerosol are sucked through a cooling system by applying a reduced pressure. As a result of this, the particles-gas stream is cooled to approx. 100 to 160 °C. The solid is separated off from the waste gas stream in a cyclone.
The pyrogenically prepared silica doped with aluminium oxide by means of aerosol is obtained as a white finely divided powder. In a further step, still adhering hydrochloric acid residues are removed from the silica by treatment with air containing steam at elevated temperature.
The BET surface area of the pyrogenic silica doped with aluminium oxide by means of aerosol is 203 m2/g.
The preparation conditions are shown in table 1. Further analytical data of the silica which can be employed according to the invention are given in table 2.
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Figure 2 shows an EM photograph of the pyrogenic silica doped with aluminium oxide by means of aerosol according to example 1.
5 It is noticeable that there are many individual spherical primary particles which have not coalesced with one another.
The difference between the pyrogenic silicas which are doped with aluminium oxide by means of aerosol and can be 10 employed according to the invention and pyrogenic silicas of known preparation and the same specific surface area manifests itself in particular in the DBP absorption, which is a measure of the structuring of the pyrogenic silica (i.e. of the degree of coalescence thereof).
The commercially obtainable silica OX 50 prepared by the pyrogenic high-temperature flame hydrolysis process thu s has (at a BET surface area of 50 m2/g) a DBP absorption of approx. 160 (g/100g), while the pyrogenic silica which is doped with 0.187 wt.o A1203 and can be employed according to the invention has a DBP absorption of only 81 (g/100g).
The consequence of the very low DBP absorption is that dispersions of low viscosity can be prepared from the pyrogenic silica doped with aluminium oxide. Dispersions with a high degree of filling with solid are easy to prepare because of these properties.
Mixtures of the silicas which can be employed according to the invention with other pyrogenically prepared or precipitated silicas or bentonites or other conventional fillers for the preparation of polyesters are in principle also possible.
Example 3 Dispersion of--the silica in ethylene glycol Ethylene glycol, which is a starting material for the production of polyester fibres, is mixed with silicon dioxide doped with aluminium oxide by means of aerosol.
The dispersibility is considerably better compared with Aerosil OX50, Aerosil 50, MOX 80, A1z03 C.
A concentration of up to 60 parts per 100 parts of ethylene glycol can thus be achieved according to the invention with only a slight increase in viscosity. (Figure 4) The viscosity values determined in ethylene glycol are shown on a graph in figure 4. Figure 3 shows the particle size distribution of the various pyrogenic oxides dispersed in ethylene glycol at a concentration of 20 parts per 100 parts of ethylene glycol, and figure 4 shows the various viscosities as a function of the concentration.
According to figure 3, the silica doped with aluminium oxide by means of aerosol employed according to the invention (example 1) has the lowest average particle size of 0.14 Vim.
According to figure 4, the silica doped with aluminium oxide by means of aerosol employed according to the invention (example 1) has the lowest increase in viscosity.
Polyesters are known compounds which can be used inter alia for the production of textiles.
They are described in Ullmann's Encyclopedia of Industrial Chemistry vol A 21 (1992) pages 227 to 251.
The preparation of polyester fibres is known from Ullmann's Encyclopedia of Industrial Chemistry vol A 10 (1992) pages 579 to 613.
A glycol, inter alia, is employed as the alcohol in the preparation of polyesters or polyester fibres.
A filler is added to this glycol in order to establish certain physico-chemical properties of the polymer.
The invention provides polyesters, which are characterized in that they contain a silicon dioxide doped by means of aerosol.
A silicon dioxide doped with aluminium oxide by means of aerosol, such as is described in the patent application DE
19847161.0-41, can be employed as pyrogenically prepared silicon dioxide doped by means of aerosol.
The pyrogenically prepared silicon dioxide doped with aluminium oxide by means of aerosol is characterized in that the base component is a silica which is prepared pyrogenically in the manner of flame oxidation or, preferably, flame hydrolysis and is doped with a doping component of 1~10-4 and up to 20 wt.%, the amount of doping preferably being in the range from 1 to 10,000 ppm and the doping component being a salt or a salt mixture of aluminium or a suspension of an aluminium compound or 990006 FA/al metallic aluminium or mixtures thereof, the BET surface area of the doped oxide being between 5 and 600 m2/g, preferably in the range between 40 and 100 m2/g.
The doped silica can have a DBP number of less than 100g/100g.
The pyrogenically prepared silicon dioxide doped with aluminium oxide by means of aerosol can be prepared by feeding an aerosol into a flame such as is used for the pyrogenic preparation of silica in the manner of flame oxidation or, preferably, flame hydrolysis, mixing the -aerosol homogeneously with the gas mixture of the flame oxidation or flame hydrolysis before the reaction, subsequently allowing the aerosol-gas mixture to react in the flame and separating the resulting pyrogenically prepared silicas doped with aluminium oxide by means of aerosol off from the gas stream in a known manner, an aqueous solution which comprises salts or salt mixtures of aluminium or the metal itself in dissolved or suspended form or mixtures thereof being used for the preparation of the aerosol, and the aerosol being prepared by atomization by means of a two-component nozzle or by another method of aerosol preparation, preferably by an aerosol generator after ultrasonic atomization.
Salts which can be employed are: A1C13, Alz (SO9) 3, A1 (N03) 3-The processes of flame hydrolysis for the preparation of pyrogenic oxides and thus also for the preparation of silicon dioxide (silica) are known from Ullmanns Enzyklopadie der technischen Chemie [Ullmann's Encyclopaedia of Industrial Chemistry), 4th edition, volume 21, page 464.
According to the invention, mixtures of 0.1 to 100 per cent of the silicas which can be employed according to the invention with other pyrogenically prepared or precipitated 990006 FA/al silicas or bentonites or other conventional fillers in the preparation of polyesters or mixtures of these fillers can be employed.
The silica according to the invention which can be employed, which is obtained as the product, for example, using aluminium chloride salts dissolved in water for the preparation of the aerosol to be fed in, can be dispersed extremely well in polar media, such as e. g. water.
The polyester according to the invention is suitable for the production of fibres (polyester fibres). .
The invention also provides a process for the preparation of polyesters, in which glycol, preferably ethylene glycol, is esterified with an organic acid by a known route, which is characterized in that a pyrogenically prepared silicon dioxide doped by means of aerosol is added to the glycol.
The invention also provides a glycol, preferably ethylene glycol, which is characterized in that it contains a pyrogenically prepared silicon dioxide doped by means of aerosol, optionally up to max. 60 parts per part of glycol.
In a preferred embodiment of the invention, the glycol can contain the pyrogenically prepared silicon dioxide doped by means of aerosol in a concentration of 50 to 60 parts per part of glycol.
The preparation of the polyester can be carried out by a known route, such as is described in Ullmann's Encyclopedia of Industrial Chemistry, vol. A21 (1992) pages 227 to 251.
The production of the polyester fibres can be carried out by a known route, such as is described in Ullmann's Encyclopedia of Industrial Chemistry vol. A10 (1992) pages 579 to 613.
990006 FA/al According to the invention, the silicon dioxide doped with aluminium oxide by means of aerosol in the polyester fibres, which can have a diameter of 10 ~m diameter, can have an average particle size of 0.5 Vim.
The silicon dioxide according to the invention which can be employed and the process for its preparation and its use are explained and described in more detail with the aid of figure 1 and the following examples:
Figure 1 shows a diagram of the doping apparatus. The core piece of the apparatus is a burner of known construction for the preparation of pyrogenic oxides.
The burner 1 comprises the central pipe 2 which ends in the nozzle 3, from which the main gas stream flows out into the burner chamber and burns off there. The nozzle 3 is surrounded by the annular nozzle 4, out of which (ring or secondary) hydrogen flows.
In the central pipe 2 is the axial pipe 5, which ends a few centimetres before the nozzle of the central pipe 2. The aerosol is fed into the axial pipe 5.
The aerosol, which comprises an aqueous aluminium chloride solution, is produced in the aerosol generator 6 (ultrasonic atomizer).
The aluminium chloride-water aerosol produced in the aerosol generator 6 is passed by means of a light carrier gas stream through the heating zone 7, in which the water carried along evaporates, small salt crystals in finely divided form remaining in the gas phase.
Example 1 Preparation of a pyrogenically prepared silica of low BET
surface area doped with aluminium oxide by means of aerosol 990006 FA/al 5.25 kg/h SiCl9 are vaporized at approx. 130 °C and transferred into the central pipe 2 of the burner 1.
3.47 Nm3/h (primary) hydrogen and 3.76 Nm3/h air are additionally fed into the central pipe 2. 0.95 Nm3/h oxygen 5 are additionally added to this mixture.
The gas mixture flows out of the nozzle 3 of the burner 1 and burns in the burner chamber and the water-cooled flame pipe connected thereto.
0.5 Nm3/h (jacket or secondary) hydrogen and 0.3 Nm3/h nitrogen are fed into the annular nozzle 4.
Nm3/h (secondary) air are also additionally fed into the burner chamber.
The second gas stream flows out of the axial pipe 5 into the central pipe 2.
15 The second gas stream comprises the aerosol, which is produced in the aerosol generator 6 by ultrasonic atomization of A1C13 solution. The aerosol generator 6 atomizes here 460 g/h 2.29 per cent aqueous aluminium trichloride solution. The aluminium chloride aerosol is led 20 with the aid of the carrier gas of 0.5 Nm3/h air through the heated line, the aqueous aerosol being converted into a gas and a salt crystal aerosol at temperatures of approx.
180 °C.
At the burner mouth the temperature of the gas mixture (SiClq-air-hydrogen, water-aerosol) is 156 °C.
The reaction gases and the pyrogenic silica doped with aluminium oxide by means of aerosol are sucked through the cooling system by applying a reduced pressure. As a result of this, the particles-gas stream is cooled to approx. 100 to 160 °C. The solid is separated off from the waste gas stream in a cyclone.
990006 FA/al The pyrogenically prepared sil,'_ca doped with aluminium oxide by means of aerosol is obtained as a white finely divided powder.
In a further step, still adhering hydrochloric acid residues are removed from the silica by treatment with air containing steam at elevated temperature.
The BET surface area of the pyrogenic silica doped with aluminium oxide is 55 m2/g.
The preparation conditions are summarized in table 1.
Further analytical data of the silica according to the invention are given in table 2.
Example 2 Preparation of a pyrogenically prepared silica of high BET
surface area doped with aluminium oxide by means of aerosol 4.44 kg/h SiCl4 are vaporized at approx. 130 °C and transferred into the central pipe 2 of the burner 1 of known construction. 3.15 Nm3/h (primary) hydrogen and 8.2 Nm3/h air are additionally fed into the central pipe 2.
The gas mixture flows out of the nozzle 3 of the burner 1 and burns in the burner chamber and the water-cooled flame pipe connected thereto.
0.5 Nm3/h (jacket or secondary) hydrogen and 0.3 Nm3/h nitrogen are fed into the annular nozzle 4.
12 Nm3/h (secondary) air are also additionally fed into the burner chamber.
The second gas stream flows out of the axial pipe 5 into the central pipe 2.
The second gas stream comprises_the aerosol, which is produced in the separate atomizing unit 6 by ultrasonic 990006 FA/al atomization of A1C13 solution. The aerosol generator 6 atomizes here 450 g/h 2.29 per cent aqueous aluminium trichloride solution. The aluminium chloride aerosol is led with the aid of the carrier gas~of 0.5 Nm3/h air through the heated line, the aqueous aerosol being converted into a gas and a salt crystal aerosol at temperatures of approx.
180 °C.
At the burner mouth the temperature of the gas mixture (SiCl9-air-hydrogen, water-aerosol) is 180 °C.
The reaction gases and the pyrogenically prepared silica doped with aluminium oxide by means of aerosol are sucked through a cooling system by applying a reduced pressure. As a result of this, the particles-gas stream is cooled to approx. 100 to 160 °C. The solid is separated off from the waste gas stream in a cyclone.
The pyrogenically prepared silica doped with aluminium oxide by means of aerosol is obtained as a white finely divided powder. In a further step, still adhering hydrochloric acid residues are removed from the silica by treatment with air containing steam at elevated temperature.
The BET surface area of the pyrogenic silica doped with aluminium oxide by means of aerosol is 203 m2/g.
The preparation conditions are shown in table 1. Further analytical data of the silica which can be employed according to the invention are given in table 2.
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~ n, O
N -r-I N N ~ ,-i l0 ~ .~ r-iO -rl O N >, C1,fl~U cn O .-i .-i ~ ~ O
O .~ ~ rtirtS~ !-I
H r.>r W W t~ ~ w - EM photograph:
Figure 2 shows an EM photograph of the pyrogenic silica doped with aluminium oxide by means of aerosol according to example 1.
5 It is noticeable that there are many individual spherical primary particles which have not coalesced with one another.
The difference between the pyrogenic silicas which are doped with aluminium oxide by means of aerosol and can be 10 employed according to the invention and pyrogenic silicas of known preparation and the same specific surface area manifests itself in particular in the DBP absorption, which is a measure of the structuring of the pyrogenic silica (i.e. of the degree of coalescence thereof).
The commercially obtainable silica OX 50 prepared by the pyrogenic high-temperature flame hydrolysis process thu s has (at a BET surface area of 50 m2/g) a DBP absorption of approx. 160 (g/100g), while the pyrogenic silica which is doped with 0.187 wt.o A1203 and can be employed according to the invention has a DBP absorption of only 81 (g/100g).
The consequence of the very low DBP absorption is that dispersions of low viscosity can be prepared from the pyrogenic silica doped with aluminium oxide. Dispersions with a high degree of filling with solid are easy to prepare because of these properties.
Mixtures of the silicas which can be employed according to the invention with other pyrogenically prepared or precipitated silicas or bentonites or other conventional fillers for the preparation of polyesters are in principle also possible.
Example 3 Dispersion of--the silica in ethylene glycol Ethylene glycol, which is a starting material for the production of polyester fibres, is mixed with silicon dioxide doped with aluminium oxide by means of aerosol.
The dispersibility is considerably better compared with Aerosil OX50, Aerosil 50, MOX 80, A1z03 C.
A concentration of up to 60 parts per 100 parts of ethylene glycol can thus be achieved according to the invention with only a slight increase in viscosity. (Figure 4) The viscosity values determined in ethylene glycol are shown on a graph in figure 4. Figure 3 shows the particle size distribution of the various pyrogenic oxides dispersed in ethylene glycol at a concentration of 20 parts per 100 parts of ethylene glycol, and figure 4 shows the various viscosities as a function of the concentration.
According to figure 3, the silica doped with aluminium oxide by means of aerosol employed according to the invention (example 1) has the lowest average particle size of 0.14 Vim.
According to figure 4, the silica doped with aluminium oxide by means of aerosol employed according to the invention (example 1) has the lowest increase in viscosity.
Claims (5)
1. Polyesters, characterized in that they contain a pyrogenically prepared silicon dioxide doped by means of aerosol.
2. Polyesters according to claim 1, characterized in that they are formed as fibres.
3. Process for the preparation of polyesters according to claims 1 or 2, wherein a glykol is esterified with an organic acid by a known route, characterized in that a pyrogenically prepared silicon dioxide doped by means of aerosol is added to the glycol.
4. Glycol, characterized in that it contains a pyrogenically prepared silicon dioxide doped by means of aerosol.
5. Use of the polyester according to claim 1 for the production of polyester fibres.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19953029A DE19953029A1 (en) | 1999-11-04 | 1999-11-04 | polyester |
DE19953029.7 | 1999-11-04 |
Publications (1)
Publication Number | Publication Date |
---|---|
CA2324885A1 true CA2324885A1 (en) | 2001-05-04 |
Family
ID=7927865
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CA002324885A Abandoned CA2324885A1 (en) | 1999-11-04 | 2000-11-01 | Polyesters |
Country Status (10)
Country | Link |
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EP (1) | EP1097964A1 (en) |
JP (1) | JP3270448B2 (en) |
KR (1) | KR20010051410A (en) |
CN (1) | CN1295090A (en) |
BR (1) | BR0005241A (en) |
CA (1) | CA2324885A1 (en) |
DE (1) | DE19953029A1 (en) |
IL (1) | IL139462A0 (en) |
NO (1) | NO20005544L (en) |
TR (1) | TR200003201A2 (en) |
Families Citing this family (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2002080573A (en) * | 2000-09-05 | 2002-03-19 | Nippon Aerosil Co Ltd | Raw material dispersion for production of polyester, method for producing the same and method for producing polyester product by using the same dispersion |
DE10239144A1 (en) * | 2002-08-27 | 2004-03-18 | Degussa Ag | dispersion |
DE10258857A1 (en) * | 2002-12-17 | 2004-07-08 | Degussa Ag | Fumed silica and dispersion thereof |
ATE406405T1 (en) * | 2005-06-25 | 2008-09-15 | Evonik Degussa Gmbh | THERMOPLASTIC MATRIX CONTAINING SILANIZED PYROGENIC SILICIC ACID |
KR101696926B1 (en) * | 2016-05-27 | 2017-01-17 | 라이트웍스 주식회사 | Frame synchronizing apparatus for passive optical network and method thereof |
Family Cites Families (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE2633358C2 (en) * | 1976-07-24 | 1986-10-30 | Hoechst Ag, 6230 Frankfurt | Use of polyethylene terephthalate for the production of stretched films |
JPS60246813A (en) * | 1984-05-16 | 1985-12-06 | Teijin Ltd | Production of ultrafine polyester yarn |
JPH03134052A (en) * | 1989-10-18 | 1991-06-07 | Toyobo Co Ltd | Orientated polyester film |
FR2658840B1 (en) * | 1989-12-20 | 1994-02-11 | Rhone Poulenc Fibres | PROCESS FOR OBTAINING PET YARNS WITH BETTER PRODUCTIVITY. |
DE19650500A1 (en) * | 1996-12-05 | 1998-06-10 | Degussa | Doped, pyrogenic oxides |
DE19847161A1 (en) * | 1998-10-14 | 2000-04-20 | Degussa | Fumed silica doped with aerosol |
-
1999
- 1999-11-04 DE DE19953029A patent/DE19953029A1/en not_active Ceased
-
2000
- 2000-09-27 EP EP00120967A patent/EP1097964A1/en not_active Withdrawn
- 2000-11-01 JP JP2000334566A patent/JP3270448B2/en not_active Expired - Fee Related
- 2000-11-01 CA CA002324885A patent/CA2324885A1/en not_active Abandoned
- 2000-11-01 TR TR2000/03201A patent/TR200003201A2/en unknown
- 2000-11-02 KR KR1020000064941A patent/KR20010051410A/en not_active Application Discontinuation
- 2000-11-03 IL IL13946200A patent/IL139462A0/en unknown
- 2000-11-03 CN CN00133412A patent/CN1295090A/en active Pending
- 2000-11-03 NO NO20005544A patent/NO20005544L/en not_active Application Discontinuation
- 2000-11-06 BR BR0005241-8A patent/BR0005241A/en not_active Application Discontinuation
Also Published As
Publication number | Publication date |
---|---|
TR200003201A3 (en) | 2001-06-21 |
NO20005544L (en) | 2001-05-07 |
CN1295090A (en) | 2001-05-16 |
EP1097964A1 (en) | 2001-05-09 |
JP2001181492A (en) | 2001-07-03 |
IL139462A0 (en) | 2001-11-25 |
BR0005241A (en) | 2001-09-18 |
KR20010051410A (en) | 2001-06-25 |
DE19953029A1 (en) | 2001-05-17 |
TR200003201A2 (en) | 2001-06-21 |
JP3270448B2 (en) | 2002-04-02 |
NO20005544D0 (en) | 2000-11-03 |
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