CN86108579A - 哺乳动物白细胞介素-4 - Google Patents
哺乳动物白细胞介素-4 Download PDFInfo
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- 229940028885 interleukin-4 Drugs 0.000 title abstract 2
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Abstract
提供了称为白细胞介素4(IL-4s)的哺乳动物蛋白及其变种蛋白,它们表现出B细胞生长因子和T细胞生长因子的活性。本发明的化合物包括天然人的和鼠的IL-4s及其变种蛋白,也包括核酸它们能与所公开的cDNA有显著同源性和/或能为哺乳动物IL-4s及其变种蛋白编码。
Description
本发明涉及多磷酸钙的制备方法。
多磷酸钙在农业上广泛用作磷酸盐肥料。
众所周知,不使用无机肥料,特别是磷肥,就不能确保农作物的高产。鉴于富磷酸盐原料资源的限制和变得枯竭的事实,人们面临的一个问题是如何利用贫五氧化二磷和含大量杂质的原料。
大多数制备浓磷肥的现有方法,包括用浓磷酸(五氧化二磷含量为50-54%)处理富磷酸盐原料(五氧化二磷含量为28-35%),在过磷酸钙室内熟化所得物料1.5~2小时,在贮存场所补充熟化产品15-20天,用石灰石中和熟化的过磷酸钙,中和的过磷酸钙进行造粒和干燥,冷却干燥的颗粒,(Kopylov等,苏联,莫斯科,1976年,双料过磷酸钙)。上述工艺技术需要用富五氧化二磷酸盐原料,长时间熟化过磷酸钙,并半随着释放出氟气,最后,中和熟化的过磷酸钙。
美国田纳西州流域管理局(美国专利号3,208,821,分类号23-109 1965,9,28)过磷酸钙的制备方法在于用浓磷酸(含五氧化二磷52-54%)分解天然磷酸盐,以产生浓过磷酸钙,使这种过磷酸钙熟化三十天,在66℃温度下造粒与干燥1小时,在干燥器内,以3-7℃分的升温速率缓慢并均匀地加热到204-302℃。
此法需要用浓磷酸,在贮存场所长期熟化,而在干燥器内缓慢并均匀加热的过程是难以实现的。
已经了解有几种方法由贫五氧化二磷和含有大量杂质(氧化镁3%,二氧化二铁2%,三氧化二铝2%)(例如,苏联发明者的执照号,1981年,8811093)的磷酸盐原料,制备多磷酸钙。这种方法在于用弱萃取磷酸处理磷酸盐原料,所得浆液在250-320℃温度下干燥,然后,干燥产物在1200℃下熔融,熔体注入水中进行淬火,成品的五氧化二磷含量为57.2%。
根据以上方法制备多磷酸钙的工艺是多级的,因此需要高温熔融和耐腐蚀及耐热的设备。
按照苏联发明者1965年执照号179284,从贫五氧化二磷含量的磷酸盐原料制备过磷酸钙的方法也是已知的生产工艺。此法,用磷酸和硫酸的混合物处理盐原料,然后,所得浆液在350-400℃温度下干燥并煅烧,继而进行造粒。上述方法得到合格的产品,其五氧化二磷含量(重量%)为:
普通的 五氧化二磷 28-37
可吸收的 五氧化二磷 26-35
水溶性的 五氧化二磷 0.2-0.8
这种生产工艺可以从贫磷酸盐原料获得磷酸盐肥料,免除了需要高温的熔融阶段。然而,用这种方法,合格产品的产率是不够高的,只达到10-12%,此外,可吸收的和含水的五氧化二磷含量也是小的。
因此,从富磷酸盐原料制备多磷酸钙的现有方法,一般是多级的,需要用浓磷酸。从贫磷酸盐原料获得合格产品,包括使用高温和专门设备。当制备多磷酸钙的工艺是在缓和的条件下进行时,目标产品的产率是不够高的,不同形式五氧化二磷的含量也是不显著是的。
本发明目的在于多磷酸盐钙制备方法的措施,即,利用简单的技术,使这种方法有可能获得足够高的产率的多磷酸钙和含有不同形式的五氧化二磷。
由于对制备多磷酸钙在方法上的措施结果,上述目的能够达到。这种方法包括用磷酸与硫酸的混合物,在80-110℃温度下处理磷酸盐原料,干燥所得浆液,造粒和煅烧。在这个工艺过程中,根据本发明,浆液的干燥和造粒在140-200℃温度下进行。接着,在260-320℃温度下煅烧干燥产品。
因此,可以使用富原料(含五氧化二磷28-39%)和浮选精矿或含有大量杂质(例如氧化镁3~5,%氧化铁2-3%,三氧化二铝2-3%,二氧化硅10-30%)的贫(五氧化二磷20-25%)磷酸原料。
根据本发明的方法,为了处理磷酸原料,可以使用含有大量杂质的萃取磷酸;不需要涉及有许多技术困难的酸的浓缩过程。
在处理磷酸盐原料的过程中,使用硫酸可以提高后期的分解度。这样的处理过程,生成的磷酸钙是多磷酸钙的有价值组份,它有利于中和酸性土壤,并向土壤提供硫。
干燥和造粒所选择的温度范围,确保从浆液中除去部分水份,在这些情况下,含有大量水分的粒状浆液,用喷射方法,沉积在干颗粒上,于是,颗粒被干燥及强化。在干燥及造粒过程中,浆液在140℃以下时会生成性能不够满意的粒料:它们的特点是提高了产品的酸度和湿度(分别为12%和5%)。浆液在200℃以上时,造粒与干燥导致产品中可销售的粒级减少,灰份含量增加。
如果粒料在260℃以下煅烧,则产品游离的五氧化二磷含量增加(6~8%),而需要中和。如果在320℃以上煅烧,水溶性五氧化二磷含量则发生急剧下降。
为了增加多磷酸钙中普通的及水溶性的五氧化二磷含量,并为精确控制上述形式的无氧化二磷含量提供可能性,建议在硫酸铵(P2O5∶SO3=3-30∶1)存在的情况下,用上述的酸处理磷酸盐原料。
与浆液组分起反应的硫酸铵,促进形成水溶性形式的五氧化二磷。硫酸铵是炼焦化学和氨与己内酰胺生产的废料。
引入少量的硫酸铵,即在上述引用的最少量以下,在多磷酸钙中水溶性五氧化二磷含量得不到有效的提高。如果引入的硫酸铵大于上述引用量的上限,则产品中的普通五氧化二磷含量下降。
在这里推荐的多磷酸钙的制备方法,既能使用富又能使用贫五氧化二磷两种磷酸盐原料,并可制备含硫的浓磷肥,这种肥料具有长效性以及氟含量低的特点。
通过改变磷酸和硫酸(为处理磷酸盐原料而用)的比例和改变造粒与干燥的温度以及煅烧粒料的温度,可以制备为特定作物和/或土壤需要的含有可吸收和水溶形式的五氧化二磷的肥料,
按照本方法制备的多磷酸钙,兼有普通过磷酸钙和双料过磷酸钙的最佳性能:类似于普通过磷酸钙,它含有促进土壤石灰中和的亚硫酸钙(20~25%),而且也是硫的来源;类似于双料过磷酸钙,它含有可吸收的五氧化二磷40~50%,这就是浓磷肥。
这种肥料的氟含量(0.3~0.5%)比普通过磷酸钙或双料过磷酸钙的氟含量(1.5~3.0%)小得多。所以,使用上述肥料在土壤中积聚的氟较少。
本方法与先有技术相比,有可能使煅烧温度降低到260-320℃,普通五氧化二磷含量提高到42-54%,水溶性五氧化二磷含量提高到10-36%。成粒产品的产率也可以提高到70-85%。
本方法制备多磷酸盐,在技术上是简单的,并能用下列方法加以实现。
将磷酸和硫酸装入如化学反应器或装有搅拌器的圆柱体容器内,所得混合物加热到80-100温度,然后,在其中加入磷酸盐原料。将容器内的物料搅拌0.5-1小时,按此法制得的浆液,用喷嘴喷射在温度为140-200℃的干燥和造粒的设备上,例如,喷在转鼓式造粒机、干燥器和流化床的烘箱上。在这些条件下,浆液成粒并同时干燥。干燥的产品,在260-320℃温度下,在煅烧设备上煅烧,冷却煅烧产品。
在使用硫酸铵的情况下,硫酸铵与磷酸盐原料同时加入。
本方法制备磷酸钙能连续进行。在工业规模上,在连续的工艺条件下,将酸、磷酸盐原料,如果需要,还有硫酸铵物料,连续装入装有搅拌器的反应器内,浆液的产率是这样控制,其结果,磷酸盐原料的分解需要1小时。成粒、干燥和煅烧过程是在适当的设备上连续进行的。
为了更好地理解本发明,下面给出其实施方案的具体的实施例作为举例说明。
实施例1
将342.1份重含有五氧化二磷浓度为22.4%的萃取磷酸和26.5份重浓度为92.5%的硫酸,注入装有搅拌器的反应器内,所得混合物加热到100℃。然后,加入100份重含五氧化二磷20%的粒状亚磷酸盐,在上述温度下搅拌反应器内的物料0.5~1小时,用喷嘴将所得浆液喷射到160℃温度的转鼓式造粒机和干燥器上。干燥的产品在260℃温度下煅烧,所得产品的主要组分含量(重量%)为:
普通 五氧化二磷 44
可吸收的 五氧化二磷 40
游离的 五氧化二磷 4
水溶性的 五氧化二磷 20
五氧化二硫 13
氟 0.5
粒状产品(1-4毫米的粒级)的产率为70%。
实施例2
除了磷酸盐原料含五氧化二磷24.5%,在200℃温度下进行造粒与干燥,煅烧在320℃温度下进行以外,在实施例1特定的条件下制备多磷酸钙。所得产品,根据其主要组分具有下列组成:
普通的 五氧化二磷 48
可吸收的 五氧化二磷 42
水溶性的 五氧化二磷 10
游离的 五氧化二硫 2
三氧化硫 14
氟 0.3
1-4毫米的粒状产品的产率为80%
实施例3
除了混酸加热到90℃,磷酸盐原料含五氧化二磷29%,磷酸和硫酸的量分别为210份和30份重,在140℃温度下造粒和干燥,在300℃温度下煅烧以外,在实施例1描述的条件下制备多磷酸钙。
产物具有以下组成(主要组分,重量%)
普通的 五氧化二磷 46
可吸收的 五氧化二磷 43
水溶性的 五氧化二磷 15
游离的 五氧化二硫 3
三氧化硫 15
氟 0.4
1-4毫米粒状产品的产率为85%
实施例4
除了混酸加热到80℃,磷酸盐原料含有五氧化二磷39.4%,磷酸与硫酸分别为200份重和36份重,在150℃温度进行造粒与干燥,在320℃温度下进行煅烧以外,在如实施例1描述的条件下,制备多磷酸钙。
产物具有以下组成(主要组分,重量%)
普通的 五氧化二磷 45
可吸收的 五氧化二磷 41
水溶性的 五氧化二磷 20
游离的 五氧化二硫 4
三氧化硫 16
氟 0.4
1-4毫米粒状产品的产率为80%。
实施例5
把294份重的磷酸和16.1份重的硫酸装入装有搅拌器的反应器内,将此混合物加热到80℃,然后,在其中加入100份重含有五氧化二磷24.5%的磷酸盐原料,将物料搅拌0.5小时。接着,把12份重的硫酸铵加到混合物中,后者再搅拌0.5小时。五氧化二磷和三氧化硫的比例为三比一。
浆液在160℃温度下造粒,粒料在300℃温度下煅烧。
产物具有以下组成(主要组分,重量%)
普通的 五氧化二磷 42.0
可吸收的 五氧化二磷 41.0
水溶性的 五氧化二磷 26.7
游离的 五氧化二硫 2.2
三氧化硫 8.0
氟 0.3
氮 1.0
实施例6
除了344份重磷酸,9.8份重的硫酸,17.2份重的硫酸铵之外,多磷酸钙在实施例5描述的条件下制备。
五氧化二磷和三氧化硫的比例为四比一。
产物具有以下组成(主要组分,重量%)
普通的 五氧化二磷 42.8
可吸收的 五氧化二磷 41.3
水溶性的 五氧化二磷 28.6
游离的 五氧化二硫 3.2
三氧化硫 11.0
氟 0.2
氮 1.5
实施例7
除了420份重的磷酸,20份重的硫酸铵,浆液的造粒与干燥在140℃温度下进行,并在320℃温度下煅烧粒料之外,多磷酸钙在实施例5描述的条件下制备。
五氧化二磷与三氧化硫的比例为八比一。
产物具有以下组成(主要组分,重量%)
普通的 五氧化二磷 49.9
可吸收的 五氧化二磷 48.5
水溶性的 五氧化二磷 36.6
游离的 五氧化二硫 4.0
三氧化硫 8.0
氟 0.2
氮 2.0
实施例8
除了420份重的磷酸,5份重的硫酸铵,在140℃温度下造粒与干燥,在320℃温度下进行煅烧之外,多磷酸钙在实施例5描述的条件下制备。
五氧化二磷与三氧化硫的比例为三十比一。
产物具有以下组成(主要组分,重量%)
普通的 五氧化二磷 54.0
可吸收的 五氧化二磷 50.0
水溶性的 五氧化二磷 9.2
游离的 五氧化二硫 1.0
三氧化硫 2.0
氟 0.3
氮 0.5
Claims (2)
1、多磷酸钙的制备方法,包括用磷酸和硫酸混合物在80-100℃温度下处理磷酸盐原料,干燥所得浆液,并进行造粒与煅烧几个阶段,其特征在于浆液及其造粒在140-200℃温度下进行,继而在260-320℃温度下煅烧所得产品。
2、根据权利要求1的方法,其特征在于在硫酸铵
(P2O5∶SO3=3-30∶3)存在的情况下,用上述酸处理磷酸盐原料。
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1987
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- 1987-07-16 DK DK371087A patent/DK371087A/da not_active Application Discontinuation
- 1987-07-17 NO NO872988A patent/NO301234B1/no not_active IP Right Cessation
- 1987-07-17 OA OA59167A patent/OA08947A/xx unknown
- 1987-08-10 MY MYPI87001250A patent/MY101972A/en unknown
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1991
- 1991-12-30 CZ CS914141A patent/CZ414191A3/cs unknown
- 1991-12-30 SK SK4141-91A patent/SK414191A3/sk unknown
-
1993
- 1993-01-21 KR KR1019930000857A patent/KR940007773B1/ko not_active IP Right Cessation
-
1995
- 1995-08-25 JP JP7217072A patent/JP2568394B2/ja not_active Expired - Lifetime
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1996
- 1996-09-30 GR GR960402553T patent/GR3021198T3/el unknown
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1998
- 1998-06-02 HK HK98104741A patent/HK1005594A1/xx not_active IP Right Cessation
- 1998-07-29 HK HK98109519A patent/HK1008823A1/xx not_active IP Right Cessation
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