WO1991001349A1 - Procede pour la fabrication d'une charge destinee a des matieres moulables en pvc, utilisation de la charge ainsi obtenue et matiere moulable en pvc la renfermant - Google Patents

Procede pour la fabrication d'une charge destinee a des matieres moulables en pvc, utilisation de la charge ainsi obtenue et matiere moulable en pvc la renfermant Download PDF

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Publication number
WO1991001349A1
WO1991001349A1 PCT/EP1990/001176 EP9001176W WO9101349A1 WO 1991001349 A1 WO1991001349 A1 WO 1991001349A1 EP 9001176 W EP9001176 W EP 9001176W WO 9101349 A1 WO9101349 A1 WO 9101349A1
Authority
WO
WIPO (PCT)
Prior art keywords
filler
acid
mixture
temperatures
pvc
Prior art date
Application number
PCT/EP1990/001176
Other languages
German (de)
English (en)
Inventor
Franz Wirsching
Rolf HÜLLER
Albert W. PÜRZER
Michael Rosenthal
Original Assignee
Robaco Chemie Handelsgesellschaft Mbh
Gypsum Research, S.A.
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority claimed from DE19893923934 external-priority patent/DE3923934A1/de
Priority claimed from DE19893940471 external-priority patent/DE3940471A1/de
Application filed by Robaco Chemie Handelsgesellschaft Mbh, Gypsum Research, S.A. filed Critical Robaco Chemie Handelsgesellschaft Mbh
Publication of WO1991001349A1 publication Critical patent/WO1991001349A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/02—Compounds of alkaline earth metals or magnesium
    • C09C1/025—Calcium sulfates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B11/00—Calcium sulfate cements
    • C04B11/05—Calcium sulfate cements obtaining anhydrite, e.g. Keene's cement
    • 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
    • C08K3/30—Sulfur-, selenium- or tellurium-containing compounds

Definitions

  • Calcium sulfate which has been produced by an annealing process by prolonged heating to about 300 ° C, is known as a filler for PVC molding compositions. It will
  • Calcium sulfate produced is still active, i.e.
  • the first step is calcium sulfate anhydrite III
  • EP-A-0 237 802 describes a method for
  • PVC moldings observed undesirable discoloration, which cannot be tolerated in particular in the case of hard PVC moldings, for example for window profiles.
  • suitable filler based on calcium sulfate anhydrite II for PVC molding compositions can be obtained by a process in which finely divided calcium sulfate dihydrate is moistened with a dehydrating, dilute acid and the mixture is subjected to a heat treatment at elevated temperatures
  • PVC molding compounds for example in the case of soft PVC for the production of light-colored cables, can be achieved.
  • Amounts of acid are therefore preferred. up to 3 wt .-% used.
  • the amount of acid are therefore preferred. up to 3 wt .-% used.
  • Humidity levels lower than 5% by weight are technically less suitable for the process.
  • the heating in the method according to the invention in embodiment (a) is advantageously carried out by direct firing or by rapid heating by means of indirect heat exchangers with a relatively high level
  • Temperature and acidity Will at low Temperatures, e.g. 80 to 110 ° C annealed, require longer annealing times, preferably 2.5 to 24 hours. If the temperature is between 150 and 190 ° C, times between 0.3 and 0.8 hours are sufficient.
  • the process is preferably carried out in the range from 130 to 150 ° C, with an annealing time of about 0.5 to 2 hours being sufficient.
  • the tempering can also take place in the same apparatus in which the conversion of the
  • Calcium sulfate dihydrate was made in anhydrite.
  • Firing for example in a rotary kiln, a flash dryer, a spin dryer or one
  • Cyclone firing unit Direct firing can take place, for example, by burning natural gas, light heating oil, heavy heating oil or heavy oil.
  • indirectly heated rotary kilns cookers or indirectly heated trough dryers with spiral guides can be used.
  • Indirect heating can be done with hot gases, steam or
  • Heat transfer oils are carried out.
  • a particular advantage of the process according to the invention is that the moist, finely divided that is obtained in large quantities as the starting material
  • Calcium sulfate dihydrate from flue gas desulfurization (flue gas gypsum) can be used.
  • the process according to the invention can thus also be carried out in such a way that parts of the hot gases of an incineration plant with flue gas desulfurization plant are used for heating the calcium sulfate dihydrate and the exhaust gases are subsequently used in the desulfurization plant (in the case of
  • Primary particles that can be distributed with only a small grinding effort, particle sizes of less than 5 ⁇ m, preferably less than 2 ⁇ m, of the upper grain size being available.
  • the neutralization takes place by intimately mixing the still hot mixture obtained after the heating and optionally after the tempering with finely divided,
  • Calcium carbonate is preferably used for the neutralization used because there may be excess
  • PVC molding compounds have no disruptive influences.
  • the process not only evaporates the adhering water and water of crystallization, but also all of the diluted acid and removes it from the product. It is therefore generally no longer necessary to wash out or neutralize the remaining acid. Instead, it is removed from the product with the cooled hot gases. It is therefore expedient to use these exhaust gases,
  • Sulfuric acid can be converted into flue gas gypsum.
  • Another essential step in embodiment (b) is sieving, in which all particles over 90 ⁇ m, preferably over 63 ⁇ m, are removed. Such screening is possible because all the acid and adhering water have already been removed and the product is therefore not sticky and moist. Sieving makes it possible to remove disturbing and coloring impurities from the end product. While the crystals are made of pure
  • Flue gas gypsum in embodiment (b) merge into a fine, crystalline, rhombic anhydrite II, which disintegrates into particles smaller than 63 .mu.m even with low mechanical stress, the grain size of coloring and disruptive impurities remains unchanged.
  • the cooled and sieved product obtained in embodiment (b) can be dry-milled in order to obtain a high-quality filler of a desired grain size.
  • the embodiment (b) of the method according to the invention offers the advantage that flue gas gypsum of various qualities and purity levels can be used as the starting material, since it is possible to use the disruptive ones Remove contaminants, such as fly coke or fly ash. This was certainly not foreseeable, since it is known that such contaminants are built into the flue gas plaster and can normally only be removed from it again by recrystallization. In the method according to the invention, these impurities are burned, oxidized or mechanically by sieving from the
  • a masking agent or precipitant for egg ions is added.
  • the addition is preferably carried out at the time of neutralization.
  • Suitable masking agents are the agents typically used for this purpose, for example
  • Phosphates such as alkali and / or
  • E rdalkali-Hexametaphospate The addition of such masking agents reliably prevents unwanted discoloration due to the presence of iron ions.
  • the coating is preferably as
  • Dry coating is carried out, for example directly after the neutralization and / or during the
  • fatty acids and are suitable as coating agents
  • Fatty acid metal salts for example calcium stearates. With such a coating the stability of the
  • Microcrystalline calcium carbonate (champagne chalk, surface-treated, of natural origin; sales: Omya GmbH
  • the roller temperature was 190 ° Rolling time 5 min.
  • the rolled skins were subjected to a thermal stability test in accordance with DIN VDE 0472, part 614, at 200 ° C. It has been shown that both test specimens with a thermal stability of 12 min. have identical thermal stability.
  • Sample weight 37 g, kneader temperature 180oC and a speed of 60 rpm tested (Brabender Plasti-Corder).
  • the sample with the filler produced according to the invention showed an approx. 25%. Longer gel time compared to the comparison sample with calcium carbonate.
  • Example according to the invention the force recordings, measured after 3, 6 and 10 min., were approximately 4-6% lower than in the comparative example.
  • the mass temperatures were about 1 ° C lower in the example according to the invention.
  • CaCO 3 fillers were used in a PVC cable jacket recipe in the composition shown in Table 2 below.
  • Plasticizer di-iso-decyl phthalate, pre-stabilized, Hexaplas MDS; Manufacturer: ICI
  • Stabilizer / lubricant compound (basic Pb complex stabilizer or for cable extrusion;
  • the roll temperature was 180 ° C, the rolling time 5 minutes.
  • the rolled skins were subjected to an oven test at 200 ° C. to test the static thermal stability,
  • Example 4 according to the invention shows no significant difference in the thermal stability.
  • Example 3 according to the invention showed that

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

L'invention concerne un procédé pour la fabrication de matières moulables en PVC à base de sulfate de calcium-anhydrite II, dans lequel on humidifie du sulfate de calcium-dihydrate avec un acide étendu déshydratant et on soumet le mélange à un traitement thermique à température élevée. A cet effet, soit a) on soumet le mélange à un traitement thermique à des températures de 50 à 190 °C et on neutralise les acides restant dans le produit obtenu avec un carbonate alcalin et/ou alcalino-terreux, tout en extrayant l'eau résiduelle ou en formation ainsi que le gaz carbonique en formation, soit b) on chauffe le mélange à contre-courant avec un gaz chaud à des températures dépassant 350 °C, on le refroidit ensuite, on le libère, par tamisage, de toutes les particules d'un diamètre supérieur à 90 νm, de préférence à 63 νm, et on le broie éventuellement.
PCT/EP1990/001176 1989-07-19 1990-07-18 Procede pour la fabrication d'une charge destinee a des matieres moulables en pvc, utilisation de la charge ainsi obtenue et matiere moulable en pvc la renfermant WO1991001349A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
DEP3923934.9 1989-07-19
DE19893923934 DE3923934A1 (de) 1989-07-19 1989-07-19 Verfahren zur herstellung eines fuellstoffes fuer pvc-formmassen, verwendung des so hergestellten fuellstoffes und den so hergestellten fuellstoff enthaltende pvc-formmasse
DE19893940471 DE3940471A1 (de) 1989-12-07 1989-12-07 Verfahren zur herstellung von fuellstoffen
DEP3940471.4 1989-12-07

Publications (1)

Publication Number Publication Date
WO1991001349A1 true WO1991001349A1 (fr) 1991-02-07

Family

ID=25883210

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/EP1990/001176 WO1991001349A1 (fr) 1989-07-19 1990-07-18 Procede pour la fabrication d'une charge destinee a des matieres moulables en pvc, utilisation de la charge ainsi obtenue et matiere moulable en pvc la renfermant

Country Status (2)

Country Link
EP (1) EP0483193A1 (fr)
WO (1) WO1991001349A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20120165433A1 (en) * 2010-12-27 2012-06-28 Makoto Kataoka Method of producing a vinyl chloride resin formed article

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1229350A (fr) * 1968-09-26 1971-04-21
FR2445941A1 (fr) * 1979-01-08 1980-08-01 Bpb Industries Ltd Perfectionnements aux procedes et dispositifs pour traiter, par la chaleur, des materiaux fragmentes en particulier
EP0237802A1 (fr) * 1986-02-20 1987-09-23 Gebr. Knauf Westdeutsche Gipswerke KG Procédé pour la préparation de sulfate de calcium sous la forme de l'anhydrite et de sulfates de calcium durcissant

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1229350A (fr) * 1968-09-26 1971-04-21
FR2445941A1 (fr) * 1979-01-08 1980-08-01 Bpb Industries Ltd Perfectionnements aux procedes et dispositifs pour traiter, par la chaleur, des materiaux fragmentes en particulier
EP0237802A1 (fr) * 1986-02-20 1987-09-23 Gebr. Knauf Westdeutsche Gipswerke KG Procédé pour la préparation de sulfate de calcium sous la forme de l'anhydrite et de sulfates de calcium durcissant

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20120165433A1 (en) * 2010-12-27 2012-06-28 Makoto Kataoka Method of producing a vinyl chloride resin formed article
US8299145B2 (en) * 2010-12-27 2012-10-30 Tokuyama Corporation Method of producing a vinyl chloride resin formed article

Also Published As

Publication number Publication date
EP0483193A1 (fr) 1992-05-06

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